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DOE OSTI2023

Modeling the Environment-Dependent Kinetics of Oxygen Reduction Reaction – a Continuum Model for Electric Double Layer

Here, for proton-exchange-membrane fuel cells (PEMFCs) to achieve broad commercialization, improved energy-conversion efficiency with minimal Pt-based electrocatalyst is required. Because the sluggish rate of oxygen reduction reaction (ORR) limits the efficiency of PEMFCs, the efficiency improvement requires a better understanding of ORR kinetics and mechanism to design better catalyst. To understand the ORR mechanism, theoretical and experimental analyses have been conducted. While previous studies reasonably explained the catalyst-dependent activity on single crystal catalysts in 0.1 M perchloric acid solution, the explicit effect of electrolyte and related microenvironments is not thoroughly understood. The change in the electrolyte alters the electric-double-layer (EDL) structure and thus the local microenvironment at the electrode/electrolyte interface. Thus, the structure of the EDL should be carefully analyzed to uncover the electrolyte-dependent reaction kinetics. In this talk, we propose a multiscale continuum model to predict the EDL structure and examine the effect of perchloric acid concentration on ORR activity on Pt (111). The model includes Density Potential Functional Theory (DPFT) for electron density and Modified Poisson Boltzmann equation for species’ density and electric potential. Also, the interaction between adsorbents and electric field is taken into account by minimizing the grand potential. After model validation with experimentally measured double-layer capacity data as a function of applied potential and concentration, the effect of the perchloric acid concentration (0.02 M – 0.2 M) on ORR activity is analyzed and discussed. It is shown that the model reproduces the specific activity obtained in the experiments when assuming the oxygen adsorption is limiting the rate, which can be attributed to the large energetic barrier for solvent reorganization. Then, extension of the model to PEMFC ionomer electrolytes will be introduced. Overall, the model framework and findings provide insights into the ORR mechanism and guidance on how to tailor catalyst materials for increased PEMFC performance.

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2022

Low Regeneration Temperature Sorbents for Direct Air Capture of CO 2

Susteon Inc., in partnership with University of Wyoming and SoCalGas, successfully met all major technical objectives to (1) scale up the ionic liquid catalyst for amine-based sorbents for improved desorption and absorption kinetics, (2) evaluate the catalyzed amine-based sorbents for direct CO 2 capture process to determine CO 2 adsorption and desorption rates and energy requirements, and (3) based on the experimental results, develop a conceptual process design to perform a preliminary economic assessment to evaluate the potential for DAC process cost reduction using the catalyzed sorbents. Amine doped solid sorbents are effective for DAC applications and can be regenerated by heat or by a combination of heat, steam, and vacuum. The best sorbent composition identified was polyethyleneimine (PEI) on fumed silica with 200 ppm ionic liquid catalyst. This sorbent formulation was shown to have a CO 2 breakthrough capacity twice that of the non-catalyzed sorbent, in laboratory tests with air at 75% relative humidity (RH). The CO 2 adsorption rate was also 40% higher than that of the non-catalyzed sorbent. This type of sorbents has the attributes required for lowering the overall cost of DAC with high CO 2 capacity and high rate of adsorption. The combination of an industrially utilized amine-based sorbent with a highly active catalyst to form a new class of materials for DAC provides a technically viable pathway for reducing the cost of DAC to <$100/tonne of CO 2 . Laboratory measurements show that the silica/PEI (polyethyleneimine) sorbents with 100 ppm of ionic liquid catalyst have almost 100% higher CO 2 cyclic capacity and 40% higher adsorption rate. Generally, CO 2 desorption occurred at higher temperatures with a rate of desorption 10 times faster than adsorption (which occurred at ambient conditions). Therefore, adsorption rate is a much more important factor in the cost of DAC because it is directly linked to the CAPEX of the total system and the cycle time (i.e., sorbent productivity in ton/day of CO 2 captured per unit volume of the air contactor). An initial process design, coupled with techno-economic analysis, based on optimal experimental results and preliminary resulting from structured sorbent testing, showed a path to lower the DAC cost from the current cost of over $200/tonne CO 2 to less than $100/tonne with a scale-up, mature state of the technology, with projected material and process improvements. These results demonstrate the effectiveness of the catalyst in silica/PEI sorbents in enhancing sorbents’ CO 2 working capacity, in (a) increasing the rate of adsorption and desorption, and (b) in lowering the CAPEX and OPEX of the DAC system employing the ionic liquid catalyzed sorbents.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2021

Development of Antimicrobial PLA Composites for Fused Filament Fabrication

In addition to possessing the desirable properties of being a biodegradable and biocompatible polymer fabricated from renewable resources, poly (lactic acid) (PLA) has useful mechanical and thermal attributes that has enabled it to be one of the most widely-used plastics for medicine, manufacturing, and agriculture. Yet, PLA composites have not been heavily explored for use in 3D-printing applications, and the range of feasible materials for the technology is limited, which inhibits its potential growth and industry adoption. In this study, tunable, multifunctional antimicrobial PLA composite filaments for 3D-printing have been fabricated and tested via chemical, thermal, mechanical, and antimicrobial experiments. Thermally stable antimicrobial ceramics, ZnO and TiO2, were used as fillers up to 30 wt%, and poly (ethylene glycol) (PEG) was used as a plasticizer to tune the physical material properties. Results demonstrate that the PLA composite filaments exhibit the thermal phase behaviors and thermal stability suitable for 3D-printing. Additionally, PEG can be used to tune the mechanical properties while not affecting the antimicrobial efficacy that ZnO and TiO2 imbue.

TiO2↗

NASA NTRS1986

Dynamic fracture toughness

Dynamic fracture toughness versus crack velocity relations of Homalite-100, polycarbonate, hardened 4340 steel and reaction bonded silicon nitride are reviewed and discrepancies with published data and their probable causes are discussed. Data scatter in published data are attributed in part to the observed fluctuations in crack velocities. The results reaffirmed our previous conclusion that the dynamic fracture toughness versus crack velocity relation is specimen dependent and that the dynamic arrest stress intensity factor is not a unique material property.

Kobayashi, A. S.↗

NASA NTRS1989

On the nature of newly formed dust around the hydrogen-deficient star V348 Sagittarii

IUE spectra of V348 Sgr have been used to determine the extinction law from 1250 to 3080 A for circumstellar material recently ejected from it. This law differs from the standard extinction law in showing a bump at 2500 A rather than 2200 A, and in showing much lower extinction values for lambda less than 2000 A. These differences are attributed to the dust grains being formed in a hydrogen-poor environment in the case of V348 Sgr, and thus lend support to those theories of the standard extinction law which attribute its properties to the dust grains being formed in a hydrogen-rich environment.

Drilling, J. S.↗

NASA NTRS1989

Optical limiting in solutions of metallo-phthalocyanines and naphthalocyanines

Optical limiting measurements have been made on solutions of several metal containing phthalocyanines and naphthalocyanines. Measurements at 532nm using nanosecond pulses from a Q-switched Nd:YAG laser show limiting throughputs of 1-10 millijoules with mild focussing in alcohol solutions with nominal transmissions of 30-70 percent. Measurements on chloro-aluminum-phthalocyanine solutions utilizing individual 30 psec pulses or trains (spanning about 100nsec) of modelocked pulses have shown even lower limiting throughputs. Thus, the dynamic range of the limiting behavior has been shown to cover at least three orders of magnitude. Prompt limiting is attributed to strong singlet-singlet (S1-Sn) absorption, whereas the longer time limiting behavior is postulated to result from strong triplet-triplet (T1-Tn) absorption. In addition to these studies, efforts have been underway to identify materials with reduced limiting throughput and improved optical transmission characteristics.

Coulter, Daniel R.↗

NASA NTRS1995

Microcracking in composite laminates under thermal and mechanical loading

Composites used in space structures are exposed to both extremes in temperature and applied mechanical loads. Cracks in the matrix form, changing the laminate thermoelastic properties. The goal of the present investigation is to develop a predictive methodology to quantify microcracking in general composite laminates under both thermal and mechanical loading. This objective is successfully met through a combination of analytical modeling and experimental investigation. In the analysis, the stress and displacement distributions in the vicinity of a crack are determined using a shear lag model. These are incorporated into an energy based cracking criterion to determine the favorability of crack formation. A progressive damage algorithm allows the inclusion of material softening effects and temperature-dependent material properties. The analysis is implemented by a computer code which gives predicted crack density and degraded laminate properties as functions of any thermomechanical load history. Extensive experimentation provides verification of the analysis. AS4/3501-6 graphite/epoxy laminates are manufactured with three different layups to investigate ply thickness and orientation effects. Thermal specimens are cooled to progressively lower temperatures down to -184 C. After conditioning the specimens to each temperature, cracks are counted on their edges using optical microscopy and in their interiors by sanding to incremental depths. Tensile coupons are loaded monotonically to progressively higher loads until failure. Cracks are counted on the coupon edges after each loading. A data fit to all available results provides input parameters for the analysis and shows them to be material properties, independent of geometry and loading. Correlation between experiment and analysis is generally very good under both thermal and mechanical loading, showing the methodology to be a powerful, unified tool. Delayed crack initiation observed in a few cases is attributed to a lack of preexisting flaws assumed by the analysis. Some interactions between adjacent ply groups are attributed to local stress concentrations. These two effects are not captured by the analysis due to its global nature. The analysis is conservative in these cases and agrees well with data after the observed onset of cracking.

Maddocks, Jason R.↗

NASA NTRS2002

The Opposition Effect: A Very Unusual Case

The reflection of electromagnetic radiation from a planetary regolith involves a combination of geometric and physical optics processes which contribute to the signal returned to the remote observer. The geometric optics effects are the product of singly and multiply scattered radiation from the surfaces of the regolith particles, combined with radiation which has undergone various combinations of transmission through one or more regolith grains followed by one or more scatterings from other particles. The physical optics effects include diffraction of radiation around the edges of large irregular particles and cooperative coherent scattering between particles which are small when compared to the wavelength of the incident radiation. These effects produce measurable changes in the intensity and polarization of reflected light as a function of illumination and viewing geometry. In particular, as phase angle becomes small, the reflectance of a particulate material will increase non-linearly and exhibit the 'opposition effect'. In the planetary science context, the phase curve, and in particular the size of the opposition surge and the width of the phase curve near zero degrees, have been attributed to two processes commonly called 'shadow hiding' (SHOE) and 'coherent backscattering' (CBOE).

Nelson, R. M.↗

NASA NTRS2003

Creep Resistance of ZrO2 Ceramic Improved by the Addition of a Small Amount of Er2O3

Zirconia (ZrO2) has great technological importance in structural, electrical, and chemical applications. It is the crucial component for state-of-the art thermal barrier coatings and an enabling component as a solid electrolyte for solid-oxide fuel cell systems. Pure ZrO2 is of limited use for industrial applications because of the phase transformations that occur. Upon the addition of stabilizers, cubic (c-ZrO2) and tetragonal (t-ZrO2) forms can be preserved. It is the stabilized and partially stabilized forms of zirconia that function as thermal barrier coatings, solid electrolytes, and oxygen sensors and that have numerous applications in the electrochemical industry. The cubic form of ZrO2 is typically stabilized through Y2O3 additions. However, Y2O3-stabilized zirconia is susceptible to deformation at high temperatures (greater than 900 C) because of the large number of slip systems and the high oxygen diffusion rates, which result in high creep rates at high temperatures. Successful use of ZrO2 at high temperatures requires that new dopant additives be found that will retain or enhance the desirable properties of cubic ZrO2 and yet produce a material with lower creep rates. At the NASA Glenn Research Center, erbium oxide (Er2O3) was identified as a promising dopant for improving the creep resistance of. ZrO2. The selection of Er2O3 was based on the strong interactions of point defects and dislocations. Single crystals of 5 mol% Er2O3- doped ZrO2 rods (4 mm in diameter) and monofilaments (200 to 300 mm in diameter and 30 cm long) were grown using the laser-heated float zone technique, and their creep behavior was measured as a function of temperature. The addition of 5 mol% Er2O3 to single-crystal ZrO2 improved its creep resistance at high temperatures by 2 to 3 orders of magnitude over state-of-the-art Y2O3-doped crystals. Detailed microstructural characterization of ZrO2-Er2O3 single crystals has identified new mechanisms for improving the creep resistance of this class of materials. Adding Er2O3 to ZrO2 results in microstructure of stable and metastable tetragonal precipitates that with thermal treatment evolve to a tweed structure of nanosize tetragonal lamellae. The superior high-temperature creep resistance of Er2O3-doped ZrO2 is attributed to nanoscale precipitation hardening. Doping with Er2O3 will significantly increase the upper-use temperature limit of ZrO2. Potential applications include using Er2O3-doped ZrO2 as a high-temperature fiber for structural applications and adding Er2O3 to reduce the sintering rates of ZrO2 thermal barrier coatings. This work was conducted at Dpto. de F sica de la Materia Condensada, Universidad de Sevilla, Spain, and at NASA Glenn.

Martinez-Fernandez, Julian↗

NASA NTRS2010

Steady X-Ray Synchrotron Emission in the Northeastern Limb of SN 1006

We investigate time variations and detailed spatial structures of X-ray synchrotron emission in the northeastern limb of SN 1006, using two Chandra observations taken in 2000 and 2008. We extract spectra from a number of small ([approx]10'') regions. After taking account of proper motion and isolating the synchrotron from the thermal emission, we study time variations in the synchrotron emission in the small regions. We find that there are no regions showing strong flux variations. Our analysis shows an apparent flux decline in the overall synchrotron flux of [approx]4% at high energies, but we suspect that this is mostly a calibration effect, and that flux is actually constant to [approx]1%. This is much less than the variation found in other remnants where it was used to infer magnetic-field strengths up to 1 mG. We attribute the lack of variability to the smoothness of the synchrotron morphology, in contrast to the small-scale knots found to be variable in other remnants. The smoothness is to be expected for a Type Ia remnant encountering uniform material. Finally, we find a spatial correlation between the flux and the cutoff frequency in synchrotron emission. The simplest interpretation is that the cutoff frequency depends on the magnetic-field strength. This would require that the maximum energy of accelerated electrons is not limited by synchrotron losses, but by some other effect. Alternatively, the rate of particle injection and acceleration may vary due to some effect not yet accounted for, such as a dependence on shock obliquity.

Katsuda, Satoru↗

NASA NTRS2013

Radiation Shielding Optimization on Mars

Future space missions to Mars will require radiation shielding to be optimized for deep space transit and an extended stay on the surface. In deep space, increased shielding levels and material optimization will reduce the exposure from most solar particle events (SPE) but are less effective at shielding against galactic cosmic rays (GCR). On the surface, the shielding provided by the Martian atmosphere greatly reduces the exposure from most SPE, and long-term GCR exposure is a primary concern. Previous work has shown that in deep space, additional shielding of common materials such as aluminum or polyethylene does not significantly reduce the GCR exposure. In this work, it is shown that on the Martian surface, almost any amount of aluminum shielding increases exposure levels for humans. The increased exposure levels are attributed to neutron production in the shield and Martian regolith as well as the electromagnetic cascade induced in the Martian atmosphere. This result is significant for optimization of vehicle and shield designs intended for the surface of Mars.

Slaba, Tony C.↗

NASA NTRS2019

Volatile Element Depletion of the Moon – The Roles of Pre-Cursors, Post-Impact Disk Dynamics, and Core Formation

The compositional and isotopic similarity of Earth’s primitive upper mantle (PUM) and the Moon has bolstered the idea that the Moon was derived from the proto-Earth, but the Moon’s inventory of volatile lithophile elements – Na, K, Rb and Cs – are lower than in Earth’s PUM by a factor of 4 to 5. The abundances of fourteen other volatile elements exhibit siderophile behavior (volatile siderophile elements or VSE; P, As, Cu, Ag, Sb, Ga, Ge, Bi, Pb, Zn, Sn, Cd, In, and Tl) that could be used to evaluate whether the Moon was derived from the proto-Earth, and whether their depletion can be attributed to volatility or core formation. In this study, newly available core-mantle partitioning data are used, together with bulk Moon compositions, protolunar disk dynamics modelling to test the hypothesis that the Moon was derived from PUM-like material. At lunar core formation conditions, As, Sb, Ag, Ge, Bi, Sn are siderophile, whereas P, Cu, Ga, Pb, Zn, Cd, In and Tl are all weakly siderophile or lithophile. Most of the VSE can be explained by a combination of known processes – pre-cursor volatile depletion, melt-gas dynamics and equilibria in the protolunar disk, and core formation. Explaining this whole group of volatile elements may require a combination of mixing and separation of the newly formed Moon from remnant gas rich in the highest volatility VSEs. This large group of volatile elements informs a wide temperature range and offers a powerful test of melt-gas segregation mechanisms in the protolunar disk and lunar formation hypotheses.

Righter, K.↗

DOE OSTI2025

The Kinetics of the Coherent Stage of Hydroxide Corrosion on Li 2 O-Covered LiH

The capability to model LiOH growth on vacuum-baked LiH is a necessary precursor to making kinetic predictions of undesirable hydrogen outgassing from corroded LiH materials when placed in sealed-system applications. Here, in this work, LiH samples with initial LiOH surface corrosion layers less than 1.1 μm were outgassed by vacuum baking at high temperature to convert LiOH to Li 2 O. Diffuse-reflectance infrared Fourier transform (DRIFT) spectroscopy was used to measure the subsequent LiOH regrowth during exposure to 25–375 ppm of H 2 O vapor at room temperature. Logarithmic kinetics best model the growth of this coherent hydroxide corrosion layer (up to 1.5 μm) on previously vacuum-baked LiH samples. The logarithmic kinetics are attributed to the dissociation of H 2 O on the corrosion layer and the establishment of a H + /OH – electric field across the thickening LiOH corrosion layer. A time-dependent model of LiOH corrosion growth as a function of both initial LiOH thickness before vacuum baking and moisture partial pressures during re-exposure was developed to help researchers better assess the unwanted hydrogen outgassing potential from LiH/LiD materials.

Matt, Sarah M. [Lawrence Livermore National Labora↗

NASA NTRS2001

Effect of Air and Vacuum Storage on the Degradation of X-Ray-Exposed Aluminized-Teflon Investigated

Metalized Teflon FEP (fluorinated ethylene propylene, DuPont), a common thermal control material, has been found to degrade in the low-Earth-orbit space environment. The aluminized-FEP (Al-FEP) exterior layer on the Hubble Space Telescope has become extremely embrittled, with extensive cracking occurring on all sides of the telescope. This embrittlement has been primarily attributed to radiation exposure (x-rays from solar flares, electron/proton radiation, and possibly near-ultraviolet radiation) combined with thermal cycling. Limited samples of FEP tested after long-term exposure to low Earth orbit on the Hubble Space Telescope and on the Long Duration Exposure Facility indicated that there might be continued degradation in tensile properties over time. An investigation was conducted at the NASA Glenn Research Center to evaluate the effect of air and vacuum storage on the mechanical properties of x-ray-exposed FEP. Aluminized-FEP (5-mil-thick) tensile samples were x-ray exposed with 15.3-kV copper xrays for 2 hr, reducing the percent elongation to failure by approximately 50 percent in comparison to that for pristine Al-FEP. X-ray-exposed samples were stored in air or under vacuum for various time periods to see the effect of storage on tensile properties. Tensile results indicated that samples stored in air had larger decreases in tensile properties than samples stored under vacuum had, as seen in the graph. Samples stored under vacuum (for up to 400 hr) showed no further decrease in tensile properties over time, whereas samples stored in air (for up to 900 hr) appeared to show decreases in tensile properties over time. X-ray-exposed samples stored in air developed a hazy appearance in the exposed area, as seen in the photographs. When the source of the haziness was evaluated using scanning electron microscopy and atomic force microscopy, it was found to reside at the Al/FEP interface as witnessed by an increased surface roughness of the aluminized side of the material and a dramatic decrease in the adhesion between the Al and FEP. Optical properties of air-stored irradiated samples showed an increase in the diffuse reflectance, which is consistent with observed roughening that was characterized by AFM. These findings indicate that air exposure helps degrade x-ray-irradiated FEP. These results indicate that proper sample handling and storage is necessary with space-retrieved materials and with those exposed to ground-based irradiation simulation exposures.

deGroh, Kim K.↗

DOE OSTI2022

Time-dependent THMC properties and microstructural evolution of damaged rocks in excavation damage zone

Modeling coupled thermo-hydro-mechanical-chemical (THMC) processes in host rocks near high-level nuclear waste (HLW) repositories at various time scales is an extremely challenging task. The current study integrates experimental, theoretical, and numerical methods in assessing the evolution of excavation damage zone (EDZ) over time and its implication on the long-term migration of hazardous species. Argillite and rock salt and are the focus of this study. The first part of the report presents a novel time-dependent directional microcrack damage theory for generic brittle rocks. It features detailed statistical description of the microcracks within a damaged solid, permitting a direct upscaling of microscale processes such as crack growth kinetics, crack closure/opening, sliding friction to explain the macroscopic creep, nonlinear elasticity, shear dilation, and loading-unloading hysteresis. This provides a basic platform for describing the anisotropic mechanical and transport properties of damaged rocks during excavation and subsequent THMC loadings. The model is validated and numerically implemented to Finite Element (FE) package ABAQUS through the user-defined material (UMAT) interface and have demonstrated great potential in resolving the time-dependent and anisotropic evolution of damage in the EDZ. The second part of the report presents a multi-scale experimental effort in characterizing the thermal, hydraulic, and mechanical properties of Mancos shale and Avery Island salt. For the Mancos shale, triaxial compression tests are performed at different confining pressures and temperatures to probe its thermomechanical properties relevant to HLW repositories. The obtained stress-strain data are interpreted using the proposed directional damage theory. Post-test specimens are subjected to gas permeability tests to reveal the correlation between permeability and the degree of microcracking. At microscale, temperature-controlled nanoindentation tests are performed and found a linear correlation between fracture toughness and elastic modulus from 25°C to 300°C. For Avery Island salt, we have designed and manufactured a novel relative-humidity controlled uniaxial creep device. Long-term creep tests at low stresses (< 5 MPa) are performed at different levels of relative humidity (RH). Besides confirming the much higher creep rates as one would expect through extrapolating the high-stress creep data, the results reveal that the steady-state creep rate of rock salt is strongly dependent on the ambient RH, an aspect that is often neglected in the literature. Both behaviors can be attributed to the pressure-solution creep mechanism which dominates at low stress and high RH levels. The third part of the report explores a set of numerical strategies in modeling the THMC behavior of porous geomaterials. A fully implicit, monolithic FE solution that can flexibly interface with different material models and coupling mechanisms for THMC problems is developed and verified through the ABAQUS user-defined element (UEL) interface. The scheme is used to study the THM response of a hypothetical HLW storage site with reference to an existing in-situ heater test. Strategies for integrating the UEL and the microcrack UMAT are suggested. Another numerical endeavor of this study is to implement a higher-order asymptotic homogenization method to account for the heterogeneous porous structures. The same method is then extended to perform microstructure-informed thermo-mechanical modeling of generalized continua. The above outcomes of this project provide a strong thrust towards enhancing the fundamental understanding and modeling capability of the long-term evolution of host rocks in EDZ, thus helping achieve the design goal of 1-million-year isolation of high-level nuclear wastes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Laser spot welding of additive manufactured 304L stainless steel

Here, the goal of this work is to understand if an additively manufactured 304L stainless steel exhibits similar spot-welding behavior as wrought 304L stainless steel. Due to the many differences between an additively manufactured component and wrought product, it is important to determine how the material interacts with the laser and how it affects the weld bead morphology. In this paper, the laser coupling efficiency, weld size, and solidification of spot welds produced in wrought and additively manufactured 304L stainless steel were investigated. The coupling efficiency of wrought and additively manufactured 304L stainless steel of similar surface condition were approximately the same over a range of applied laser energies. Laser welding of the untreated (rougher) surface of additively manufactured 304L, however, showed improved coupling efficiency ranging between 3.3 and 100%. The rougher surface traps the incoming light and increases the coupling efficiency at lower laser energies, while at higher energy, the absorption efficiency is dominated by intrinsic absorption from the keyhole formation rather than surface roughness. The resulting spot weld microstructures differed from welds made in wrought 304L and additively manufactured 304L. Welds made in wrought 304L were fully austenitic containing what is suspected to be massive austenite, which suggests that these welds solidified as primary ferrite. Welds made in additively manufactured 304L were also fully austenitic and contained both cellular austenite and what is suspected to be massive austenite. These observations mean that welds made in additively manufactured 304L solidified as primary ferrite and primary austenite. The differences in weld microstructures made in wrought and AM 304L can be attributed to differences in the composition and solidification rate.

304L stainless steel↗

DOE OSTI2020

Nanoscale serration characteristics of additively manufactured superalloys

Structural elements made of nickel-based superalloys usually operate at high temperatures. Many surface failure mechanisms such as creep, fatigue, fretting fatigue, corrosion, and stress corrosion cracking start from the surface. Thus, studying the surface mechanical properties and deformation behavior of materials is vital in order to draw a correlation between the surface properties and failures. Herein, a nanoindentation technique was implemented to characterize surface properties of a widely used additively manufactured (AM) superalloy, i.e., Inconel 625. The specimens were tested in a range of temperatures in a vacuum chamber. Serrated plastic flow characterized by pop-in events during nanoindentation, known as Portevin-Le Chatelier (PLC) effect, was observed in all three tested elevated temperatures. This phenomenon depicts itself as bursts of plasticity in the loading section of the load-displacement curves. These bursts were studied comprehensively to explore incipient plasticity. Hertzian contact mechanics were implemented to extract the maximum shear stress beneath the indenter from the pop-in loads. The results show that the initial pop-in load increases as the temperature increases. The average initial pop-in load increases by almost four times from 300 °C to 650 °C. This was attributed to the formation of strengthening precipitates. The average size of the serrations and the magnitude of dislocation nucleation increase from 300 °C to 500 °C and decrease from 500 °C to 650 °C. Finally, the serrations are attributed to the dislocation generation and movement as well as their interaction with the solute atoms and precipitates.

36 MATERIALS SCIENCE↗

NASA NTRS1991

The effects of space radiation on thin films of YBa2Cu3O(7-x)

This investigation had two objectives: (1) to determine the effects of space radiation on superconductor parameters that are most important in space applications; and (2) to determine whether this effect can be simulated with Co-60 gamma rays, the standard test method for space materials. Thin films of yttrium barium copper oxide (YBCO) were formed by coevaporation of Y, BaF2, and Cu and post-annealing in wet oxygen at 850 C for 3.5 h. The substrate used was (100) silicon with an evaporated zirconia buffer layer. The samples were characterized by four point probe electrical measurements as a function of temperature. The parameters measured were the zero resistance transition temperature T(sub c) and the room temperature resistance. The samples were then exposed to Co-60 gamma-rays in air and in pure nitrogen, and to 780 keV electrons, in air. The parameters were then remeasured. The results are summarized. The results indicate little or no degradation in the parameters measured for samples exposed up to 10 Mrads of gamma-rays in nitrogen. However, complete degradation is preliminarily attributed to the high level of ozone generated in the chamber by the gamma-ray interaction with air. It can be concluded that: (1) the electron component of space radiation does not degrade the critical temperature of the YBCO films described, at least for energies around 800 keV and doses similar to those received by surface materials on spacecraft in typical remote sensing missions; and (2) for qualifying this and other superconducting materials against the space-radiation threat the standard test method used in the aerospace industry, namely, exposure to Co-60 gamma-rays in air, may require some further investigation. As a minimum, the sample must be either in vacuum or in positive nitrogen pressure.

Herschitz, R.↗