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All sourcesNASA NTRSDOE OSTI
NASA NTRS1972

Development of advanced material composites for use as internal insulation for LH2 tanks (gas layer concept)

A program is described that was conducted to develop an internal insulation system for potential application to the liquid hydrogen tanks of a reusable booster, where the tanks would be subjected to repeated high temperatures. The design of the internal insulation is based on a unique gas layer concept, in which capillary or surface tension effects are used to maintain a stable gas layer, within a cellular core structure, between the tank wall and the contained liquid hydrogen. Specific objectives were to select materials for insulation systems that would be compatible with wall temperatures of 350 F and 650 F during reentry into the earth's atmosphere, and to fabricate and test insulation systems under conditions simulating the operating environment. A materials test program was conducted to evaluate the properties of candidate materials at elevated temperatures and at the temperature of liquid hydrogen, and to determine the compatibility of the materials with a hydrogen atmosphere at the appropriate elevated temperature. The materials that were finally selected included Kapton polyimide films, silicone adhesives, fiber glass batting, and in the case of the 350 F system, Teflon film.

Gille, J. P.↗
NASA NTRS1974

Isotopic composition of lithium, potassium, rubidium, and strontium in lunar surface material

The isotopic composition of alkali and alkaline earth elements in the Luna 16 regolith was investigated by the method of thermionic emission, without chemical separation. The isotopic composition of the lithium in two regolith samples did not differ (within the limits 0.5 percent) from the mean of the terrestrial reference standard. At the same time, the observed difference (1 percent) in the isotopic composition of lithium between the samples requires further investigation and confirmation. The isotopic compositions of K and Rb did not differ within the limits of experimental error from the isotopic composition of the reference standard.

Zaslavskiy, V. G.↗
NASA NTRS1975

Compositional effects on mechanical properties of hafnium-carbide-strengthened molybdenum alloys

The mechanical properties of swaged rod thermomechanically processed from arc melted Mo-2Re-Hf-C alloys containing as much as 0.9-mol% HfC were evaluated. The low-temperature ductilities of these alloys were not influenced by the amount of HfC present but by the amount of Hf in excess of stoichiometry. Maximum ductility occurred at 0.2- to 0.3-at.% excess Hf. At 0.3- to 0.5-mol% HfC, alloy strength varied directly with the Mo content of extracted carbide particles, both decreasing as the amount of excess Hf increased. Additions of 2-at.% Re had little effect on strength or ductility. Tensile and creep strengths of Mo-2Re-0.7Hf-0.5C alloy equaled or exceeded those of other high strength Mo alloys.

Witzke, W. R.↗
NASA NTRS1974

The role of nickel content and the magnetic remanence in iron-nickel alloys of lunar composition

Lunar samples are magnetic primarily due to the body centered cubic (BCC) iron and iron-nickel alloys they contain. Presented for the first time are results which demonstrate that the magnitude of the martensitic thermal remanence (MTRM) induced on quenching iron-nickel alloy in the geomagnetic field depends on the nickel content of the alloy. High magnetic stability is due to the increasing dislocation density and increasingly complex microstructures associated with increasing nickel content in the alloys. The results agree with the mechanical and structural properties of the alloys. The characteristic quench martensite microstructure observed on metallographic examination provides a recognition criterion for the MTRM mechanism. These results are important for lunar and meteoritic research intending to ascertain the paleofield responsible for the observed remanent magnetization.-

Wasilewski, P.↗
NASA NTRS1976

Composition effects on mechanical properties of HfC-strengthened molybdenum alloys

The mechanical properties of swaged rod thermomechanically processed from arc-melted Mo-2Re-Hf-C alloys containing as much as 0.9 mol pct HfC have been evaluated. The low temperature ductilities of these alloys were not influenced by the amount of HfC present but by the amount of Hf in excess of stoichiometry. Maximum ductility occurred at 0.2 to 0.3 at. pct excess Hf. At 0.3 to 0.5 mol pct HfC, alloy strength varied directly with the Mo content of extracted carbide particles, both decreasing as the amount of excess Hf increased. Additions of 2 at. pct Re had little effect on strength or ductility. Tensile and creep strengths of Mo-2Re-0.7Hf-0.5C alloy equaled or exceeded those of other high strength Mo alloys.

Witzke, W. R.↗
NASA NTRS2011

Material Characterization and Geometric Segmentation of a Composite Structure Using Microfocus X-Ray Computed Tomography Image-Based Finite Element Modeling

This study utilizes microfocus x-ray computed tomography (CT) slice sets to model and characterize the damage locations and sizes in thermal protection system materials that underwent impact testing. ScanIP/FE software is used to visualize and process the slice sets, followed by mesh generation on the segmented volumetric rendering. Then, the local stress fields around several of the damaged regions are calculated for realistic mission profiles that subject the sample to extreme temperature and other severe environmental conditions. The resulting stress fields are used to quantify damage severity and make an assessment as to whether damage that did not penetrate to the base material can still result in catastrophic failure of the structure. It is expected that this study will demonstrate that finite element modeling based on an accurate three-dimensional rendered model from a series of CT slices is an essential tool to quantify the internal macroscopic defects and damage of a complex system made out of thermal protection material. Results obtained showing details of segmented images; three-dimensional volume-rendered models, finite element meshes generated, and the resulting thermomechanical stress state due to impact loading for the material are presented and discussed. Further, this study is conducted to exhibit certain high-caliber capabilities that the nondestructive evaluation (NDE) group at NASA Glenn Research Center can offer to assist in assessing the structural durability of such highly specialized materials so improvements in their performance and capacities to handle harsh operating conditions can be made.

Abdul-Aziz, Ali↗
DOE OSTI2017

Development of Computational Tools for Modeling Thermal and Radiation Effects on Grain Boundary Segregation and Precipitation in Fe-Cr-Ni-based Alloys

This work aims at developing computational tools for modeling thermal and radiation effects on solute segregation at grain boundaries (GBs) and precipitation. This report described two major efforts. One is the development of computational tools on integrated modeling of thermal equilibrium segregation (TES) and radiation-induced segregation (RIS), from which synergistic effects of thermal and radiation, pre-existing GB segregation have been taken into consideration. This integrated modeling was used in describing the Cr and Ni segregation in the Fe-Cr-Ni alloys. The other effort is thermodynamic modeling on the Fe-Cr-Ni-Mo system which includes the major alloying elements in the investigated alloys in the Advanced Radiation Resistant Materials (ARRM) program. Through thermodynamic calculation, we provide baseline thermodynamic stability of the hardening phase Ni2(Cr,Mo) in selected Ni-based super alloys, and contribute knowledge on mechanistic understanding on the formation of Ni2(Cr,Mo) in the irradiated materials. The major outcomes from this work are listed in the following: 1) Under the simultaneous thermal and irradiation conditions, radiation-induced segregation played a dominant role in the GB segregation. The pre-existing GB segregation only affects the subsequent radiation-induced segregation in the short time. For the same element, the segregation tendency of Cr and Ni due to TES is opposite to it from RIS. The opposite tendency can lead to the formation of W-shape profile. These findings are consistent with literature observation of the transitory W-shape profile. 2) While TES only affects the distance of one or two atomic layers from GBs, the RIS can affect a broader distance from GB. Therefore, the W-shape due to pre-existing GB segregation is much narrower than that due to composition gradient formed during the transient state. Considering the measurement resolution of Auger or STEM analysis, the segregation tendency due to RIS should play a dominant role in the measured values. However, The GB segregation due to pre-existing GB segregation may affect the chemical potential of element at GB, and subsequently the corrosion resistance. 3) Based on the newly developed thermodynamic database of Fe-Cr-Ni-Mo, we predicted the Ni2(Cr,Mo) as a thermodynamically stable phase in all investigated low Fe-content Ni-based alloys. The calculated phase amount decreases with the increasing Fe content, being consistent with that observed in the irradiated materials. 4) The formation of the Ni2(Cr,Mo) phase in irradiated materials is due to irradiation enhanced diffusion. The calculated equilibrium Ni2(Cr,Mo) amount is more than that observed in the irradiated materials, suggesting that the amount of Ni2(Cr,Mo) is likely to increase more with further irradiation.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Laser metal deposition of refractory high-entropy alloys for high-throughput synthesis and structure-property characterization

Progress in materials development is often paced by the time required to produce and evaluate a large number of alloys with different chemical compositions. This applies especially to refractory high-entropy alloys (RHEAs), which are difficult to synthesize and process by conventional methods. To evaluate a possible way to accelerate the process, high-throughput laser metal deposition was used in this work to prepare a quinary RHEA, TiZrNbHfTa, as well as its quaternary and ternary subsystems by in-situ alloying of elemental powders. Compositionally graded variants of the quinary RHEA were also analyzed. Our results show that the influence of various parameters such as powder shape and purity, alloy composition, and especially the solidification range, on the processability, microstructure, porosity, and mechanical properties can be investigated rapidly. The strength of these alloys was mainly affected by the oxygen and nitrogen contents of the starting powders, while substitutional solid solution strengthening played a minor role.

additive manufacturing↗
DOE OSTI2019

Development of an Electrochemical Impedance Instrument for Monitoring Corrosion Formation (Oxide and Hydride) on Cladding Materials

The objective of this work package is to develop electrochemical impedance spectroscopic (EIS) techniques for the in pile measurement of changes in cladding materials in coupling with model simulation and material characterization. This work package will involve the initial development of electrochemical sensing technologies for measuring spatial and time resolved changes in cladding chemistry. Specific attention will be paid to monitoring changes in monitor cladding corrosion including oxide and hydride formation and deformation. The planned work during this period was focused on cladding material zirconium alloy corrosion, oxide and hydride development, and to characterize samples using EIS under controlled gas atmosphere, atom probe tomography (APT), Raman Spectroscopy, and Synchrotron X-ray diffraction (XRD). The corrosion, including oxide and hydride of zirconium alloy samples, was tested in this study. The samples were treated at a gas environment containing 3% H2 (vol%) balanced with N2 gas at various temperatures (100 – 500°C) and different times (up to 60 hours) and were characterized by in situ EIS. After treatment, various characterization techniques were applied to measure the samples, including TGA, Ramen, XRD, and APT. This study found that impedance spectra can be affected significantly with (furnace/environment) temperature. Higher temperature resulted in higher overall impedance, and longer exposure time exerted similar effects. Proof of concept characterization of oxidized samples, including TGA, Raman, XRD, and APT, were accomplished on samples exposed to 700 oC gas environment containing 20% O2 and 80% N2. TGA provides observable breakaway and bulk oxide growth measurements. High-temperature, in-situ Raman provides observation of oxidation stress at the surface of the oxide. Additionally, a transition from tetragonal to monoclinic zirconia can be seen early in the oxidation experiment. Specifically, tetragonal-rich zirconia is seen at the metal/oxide interface, where a transition to monoclinic-rich zirconia is seen in the bulk of the oxide. It has also been confirmed that highly compressive residual stresses are seen near the metal/oxide interface. It is concluded that the transition from tetragonal to monoclinic zirconia is induced by massive shifts in stress as the oxide grows. APT has supplied evident differences in the distribution of zirconium and oxygen at the metal/oxide interface. On the pre-breakaway sample, the metastable Zr(O) region at the boundary is relatively thin, interfaced by Zr-rich (i.e., metal) and O-rich (i.e., ZrO2) on either side. In contrast, it has been seen on a post-breakaway sample that the Zr(O) metastable region is much greater in thickness, with evidence of four “zones” showing slightly contrasting composition between 49-54% Zr. In addition, it can be seen from the Zr-2.65Nb post-breakaway sample that secondary element concentrations are considerably different than bulk composition measurements show. Specifically, Nb concentration is much lower than expected, whereas Fe concentration is much higher than expected. These differences could play a role in each element’s contribution to oxide growth mechanisms, as well as causation for breakaway. Future work is focused on analyzing EIS spectra of hydride and its correlation with characterization features, finite element (FE) modeling of cladding materials, electrochemical sensor development, targeting cladding oxides/hydrides under thermodynamic equilibria, during transients and under irradiation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2017

Magnetic nanofiber composite materials and devices using same

A nonreciprocal device is described. It includes a housing, a waveguide layer and at least one layer of magnetic nanofiber composite. The magnetic nanofiber composite layer is made up of a polymer base layer, a dielectric matrix comprising magnetic nanofibers. The nanofibers have a high aspect ratio and wherein said dielectric matrix is embedded in the polymer base layer.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Compositions for cooling materials exposed to the sun

The present invention provides for a composition comprising a pigment, wherein the composition is suitable for coating a surface that is, or is expected to be, exposed to the sun. The pigment comprises particles that fluoresce in sunlight, thereby remaining cooler in the sun than coatings pigmented with non-fluorescent particles. The particles comprise solids that fluoresce or glow in the visible or near infrared (NIR) spectra, or that fluoresce when doped. Suitable dopants include, but are not limited to, ions of rare earths and transition metals.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Enabling Multi-Material Structures of Co-Based Superalloy Using Laser Directed Energy Deposition Additive Manufacturing

Cobalt superalloys such as Tribaloys are widely used in environments that involve high temperatures, corrosion, and wear degradation. Additive manufacturing (AM) processes have been investigated for fabricating Co-based alloys due to design flexibility and efficient materials usage. AM processes are suitable for reducing the manufacturing steps and subsequently reducing manufacturing costs by incorporating multi-materials. Laser directed energy deposition (laser DED) is a suitable AM process for fabricating Co-based alloys. T800 is one of the commercially available Tribaloys that is strengthened through Laves phases and of interest to diverse engineering fields. However, the high content of the Laves phase makes the alloy prone to brittle fracture. In this study, a Ni-20%Cr alloy was used to improve the fabricability of the T800 alloy via laser DED. Different mixture compositions (20%, 30%, 40% NiCr by weight) were investigated. The multi-material T800 + NiCr alloys were heat treated at two different temperatures. These alloy chemistries were characterized for their microstructural, phase, and mechanical properties in the as-fabricated and heat-treated conditions. SEM and XRD characterization indicated the stabilization of ductile phases and homogenization of the Laves phases after laser DED fabrication and heat treatment. In conclusion, the NiCr addition improved the fabricability and structural integrity of the T800 alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Toughening materials: enhancing resistance to fracture

It has been said that ‘God invented plasticity, but the Devil invented fracture!’ Both mechanisms represent the two prime modes of structural failure, respectively, plastic collapse and the rupture/breaking of a component, but the concept of developing materials with enhanced resistance to fracture can be difficult. This is because fracture resistance invariably involves a compromise—between strength and ductility, between strength and toughness—fundamentally leading to a ‘conflict’ between nano-/micro-structural damage and the mechanisms of toughening. Here, we examine the two major classes of such toughening: (i) intrinsic toughening, which occurs ahead of a crack tip and is motivated by plasticity—this is the principal mode of fracture resistance in ductile materials, and (ii) extrinsic toughening, which occurs at, or in the wake of, a crack tip and is associated with crack-tip shielding—this is generally the sole mode of fracture resistance in brittle materials. We briefly examine how these distinct mechanistic processes have been used to toughen synthetic materials—intrinsically in gradient materials and in multiple principal-element metallic alloys with the example of metallic glasses and high-entropy alloys, and extrinsically in ceramics with the example of ceramic-matrix composites—in comparison to Nature which has been especially adept in creating biological/natural materials which are toughened by one or both mechanistic classes, despite often consisting of constituents with meagre mechanical properties. The success of Nature has been driven by its ability to cultivate the development of materials with multiple length-scale hierarchical structures that display ingenious gradients and structural adaptability, a philosophy which we need to emulate and more importantly learn to synthesize to make structural materials of the future with unprecedented combinations of mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2021

First steps toward predicting corrosion behavior of structural materials in molten salts

To address the need for physics-based models to predict corrosion behavior of materials in molten salts, here we propose potential methods to aid in selection of optimum materials for structural components in molten salt powered technologies. In the present work, the role of alloy thermodynamics and kinetics on governing corrosion rates of Ni-based alloys will be discussed combining experimental and computational methods. A few strategies are presented to quantify corrosion rates of Ni-based materials isothermally exposed in purified KCl-MgCl 2 salts at 600° C-800° C. The influence of capsule material, potential corrosion products and role of alloy composition on the observed corrosion rates was discussed with coupled thermodynamic-kinetic models. Larger depths of corrosion attack were observed in alloy 230 specimens compared to other alloys under similar conditions was attributed to the much higher chemical activity of Cr in the alloy that results in a larger Cr chemical potential gradient.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Status of Metallic Structural Materials for Molten Salt Reactors

In the US and around the world, significant interest surrounds development and deployment of nuclear systems using molten salts to transfer heat. Several configurations are being explored, including the use of fluoride salts either as the primary coolant of a reactor with solid fuel or with the fissile material dissolved in the salt. Molten Salt Reactors (MSRs) with fluoride salt typically have a thermal neutron spectrum. There are also fast-spectrum reactors that could use chloride salts to transfer heat. As a result of operation of the Molten Salt Reactor Experiment (MSRE) at Oak Ridge National Laboratory during the 1960s, a system with uranium fuel dissolved in a fluoride-salt medium is the most well-established technology. A nickel alloy with about 6%Cr and molybdenum as a solid solution strengthening agent was developed and deployed for all structural applications in this reactor. The alloy was commercialized as Hastelloy N. During these experiments and in post-decommissioning characterization of material behavior, it was determined that the most significant challenges for structural materials are embrittlement, from helium introduced by transmutation of Ni, and corrosion and grain boundary embrittlement from the fission product tellurium. The MSRE had an outlet temperature of approximately 650°C. The mechanical properties of Hastelloy N are not sufficient to support long-term operation of an MSR above this temperature. Qualification of a material for use in the ASME Boiler and Pressure Vessel Code, Section III, “Rules for Construction of Nuclear Facility Components,” Division 5, “High Temperature Reactors,” will facilitate licensing with the Nuclear Regulatory Commission. Hastelloy N has not been qualified for use in nuclear construction, and significant additional characterization would be required for Code qualification. Given that this alloy is susceptible to He embrittlement and has limited high-temperature strength, it is not recommended that Code qualification be pursued. Instead, it is recommended that a systematic development program be initiated to develop new nickel alloys that contain a fine, stable dispersion of intermetallic particles to trap He at the interface between the matrix and particle and with increased solid solution strengthening from addition of refractory elements. Extensive screening of attractive alloy compositions for elevated temperature strength, microstructural stability, weldability, and resistance to He embrittlement (characterized using ion implantation) will lead to an alloy down-selection for commercialization and Code qualification.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗