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All sources NASA NTRS DOE OSTI

NASA NTRS2003

Synthesis of Sol-Gel Precursors for Ceramics from Lunar and Martian Soil Simulars

Recent NASA mission plans for the human exploration of our Solar System has set new priorities for research and development of technologies necessary to enable a long-term human presence on the Moon and Mars. The recovery and processing of metals and oxides from mineral sources on other planets is under study to enable use of ceramics, glasses and metals by explorer outposts. We report initial results on the production of sol-gel precursors for ceramic products using mineral resources available in martian or lunar soil. The presence of SiO2, TiO2, and Al2O3 in both martian (44 wt.% SiO2, 1 wt.% TiO2,7 wt.% Al2O3) and lunar (48 wt.% SiO2, 1.5 wt.% TiO2, 16 wt.% Al2O3) soils and the recent developments in chemical processes to solubilize silicates using organic reagents and relatively little energy indicate that such an endeavor is possible. In order to eliminate the risks involved in the use of hydrofluoric acid to dissolve silicates, two distinct chemical routes are investigated to obtain soluble silicon oxide precursors from lunar and martian soil simulars. Clear solutions of sol-gel precursors have been obtained by dissolution of silica from lunar soil simular in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Similarly, sol-gel solutions produced from martian soil simulars reveal higher contents of iron oxides. The elemental composition and structure of the precursor molecules were characterized. Further concentration and hydrolysis of the products was performed to obtain gel materials for evaluation as ceramic precursors.

Sibille, L.↗

DOE OSTI2025

Continuous flow photochemical synthesis of metal–ceramic composite microparticles

We developed a UV-assisted microfluidic system to synthesize FeCrAl–Al 2 O 3 composite microparticles for additive manufacturing. Here, the system ensures precise particle size, morphology, and elemental distribution control. Increasing the dispensing pressure while keeping the oil flow rate constant resulted in larger microparticles. Laser fusing revealed FeCrAl and Al 2 O 3 phases, showing their potential as feedstocks for 3D printed heterogeneous materials such as FeCrAl/Al 2 O 3 bi-phase materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Electronic Structure, Chemical Bonding and Electrocatalytic Activity of Novel Ba(Fe0.7Ta0.3)O3-d Compounds

Ba(Fe0.7Ta0.3)O3-d (BFTO) compounds were synthesized using conventional, high-temperature solid-state ceramic reaction method by varying the sintering temperature (Ts=1200-1350 °C). The crystal structure, electronic structure and electrocatalytic activity of BFTO compounds were evaluated. Processing temperature induced phase transformations and structural quality influences the electronic structure and electrocatalytic activity of BFTO compounds. At Ts=1200 oC, Ba(Fe0.7Ta0.3)O3-d stabilizes in mixed phase of orthorhombic + rhombohedral phase (Amm2 + R3m). With increasing Ts (=1250 oC), Ba(Fe0.7Ta0.3)O3-d ceramics stabilize in tetragonal + rhombohedral [P4mm + R3m] mixed phase with a variation in the quantity of respective phases. High-resolution X-ray photoelectron spectroscopy of constituent elements, namely, Ba 3d, Fe2p, Ta 4f and O 1s reveal the electronic structure changes due to changes in chemical environment resulted from structural transformation. The electrocatalytic activity of BFTO was evaluated towards hydrogen evolution reaction (HER) and oxygen reduction reaction (ORR). Though all the samples demonstrated appreciable electrocatalytic properties, the best electrochemical catalytic activity was shown by BFTO samples sintered at 1350 °C. BFTO-1350 oC showed an onset potential of -0.690 V vs. RHE for HER and an onset potential of 0.73 V vs. RHE for ORR indicating its significant electrocatalytic performance. A general increase in activity with sintering temperature is potentially due to the improved structural quality of the BFTO ceramics. In addition to offering the fundamental insights into solid state materials based on doped BaTiO3 for electrocatalysis, the present work may contribute to the design and development of materials for high-temperature electrocatalytic converters.

Ba(Fe0.7Ta0.3)O3-d, Phase Transformation↗

DOE OSTI2022

Tritium Transport Modeling at the Pore Scale in Ceramic Breeder Materials Using TMAP8

Fusion reactors depend on the blanket material to breed and release tritium at the same rate or faster than it is consumed by the fusion reaction. Cellular ceramic breeders (CCBs) are dense materials that can maintain a high tritium breeding ratio while promoting tritium release because of highly connected pores. Assessing the tritium breeding capabilities of these materials requires a combination of extensive experimental and modeling efforts. In this work, we develop and calibrate a multiphysics model of tritium transport. This novel model accounts for ceramic and pore diffusion, trapping and detrapping, and several surface reactions at the pore surface. We perform a sensitivity analysis and calibrate the model by comparing its predictions against experimental measurements of deuterium absorption. The calibrated model is then used to model tritium absorption in samples with different pore microstructures to investigate the effect of pore interconnectivity on tritium absorption. The model is part of the development of the multiscale, multiphysics framework for tritium transport [i.e., the Tritium Migration Analysis Program (TMAP8)], which is itself built on top of the finite-element multiphysics framework multiphysics object-oriented simulation environment (MOOSE). This study demonstrates some of TMAP8’s capabilities and is the first step toward assessing the tritium breeding capabilities of ceramic breeder material designs.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2025

Correcting impedance measurements for background parasitics to characterize circuit components in cryogenic environments

Predictable circuit response is a critical prerequisite for accurate electronic measurements. Here, we describe a powerful yet straightforward experimental method and analysis model that utilizes an affordable LCR meter in conjunction with an in situ parasitic-impedance background-correction procedure to measure the temperature-dependent impedance (magnitude and phase) of up to ten individual passive circuit elements in a single cryostat run. We show how the model unambiguously identified a ∼20× drop in capacitance for 22 μF 5XR multilayer ceramic capacitors cooled from 300 K to 360 mK in an environment with a parasitic capacitance of ∼300 pF. The same experimental procedure, based on a simple two-wire measurement, was also used to measure 10 and 22 pF thin-film capacitors and 100 MΩ thick-film resistors. The results showed that the resistor values increased by up to an order of magnitude when the devices were cooled from 300 K to 360 mK. Most importantly, we showed that the simple data-acquisition method, coupled with our analysis model, enabled the measurement of component parasitics, and effectively extended the accuracy of a commercial LCR meter beyond its manufacturer-guaranteed values for a wide range of measurement frequencies. We also showed that, in the current configuration, our simple approach is limited to a capacitance accuracy of ∼10 pF.

Carpenter, R. J. [Santa Clara Univ., Santa Clara, ↗

NASA NTRS1983

Radioactive nuclear waste stabilization - Aspects of solid-state molecular engineering and applied geochemistry

Stabilization techniques for the storage of radioactive wastes are surveyed, with emphasis on immobilization in a primary barrier of synthetic rock. The composition, half-life, and thermal-emission characteristics of the wastes are shown to require thermally stable immobilization enduring at least 100,000 years. Glass materials are determined to be incapable of withstanding the expected conditions, average temperatures of 100-500 C for the first 100 years. The geological-time stability of crystalline materials, ceramics or synthetic rocks, is examined in detail by comparing their components with similar naturally occurring minerals, especially those containing the same radioactive elements. The high-temperature environment over the first 100 years is seen as stabilizing, since it can recrystallize radiation-induced metamicts. The synthetic-rock stabilization technique is found to be essentially feasible, and improvements are suggested, including the substitution of nepheline with freudenbergite and priderite for alkaline-waste stabilization, the maintenance of low oxygen fugacity, and the dilution of the synthetic-rock pellets into an inert medium.

Haggerty, S. E.↗

NASA NTRS1986

A constitutive law for finite element contact problems with unclassical friction

Techniques for modeling complex, unclassical contact-friction problems arising in solid and structural mechanics are discussed. A constitutive modeling concept is employed whereby analytic relations between increments of contact surface stress (i.e., traction) and contact surface deformation (i.e., relative displacement) are developed. Because of the incremental form of these relations, they are valid for arbitrary load-deformation histories. The motivation for the development of such a constitutive law is that more realistic friction idealizations can be implemented in finite element analysis software in a consistent, straightforward manner. Of particular interest is modeling of two-body (i.e., unlubricated) metal-metal, ceramic-ceramic, and metal-ceramic contact. Interfaces involving ceramics are of engineering importance and are being considered for advanced turbine engines in which higher temperature materials offer potential for higher engine fuel efficiency.

Plesha, M. E.↗

NASA NTRS2003

Predicting the Reliability of Ceramics Under Transient Loads and Temperatures With CARES/Life

A methodology is shown for predicting the time-dependent reliability of ceramic components against catastrophic rupture when subjected to transient thermomechanical loads (including cyclic loads). The methodology takes into account the changes in material response that can occur with temperature or time (i.e., changing fatigue and Weibull parameters with temperature or time). This capability has been added to the NASA CARES/Life (Ceramic Analysis and Reliability Evaluation of Structures/Life) code. The code has been modified to have the ability to interface with commercially available finite element analysis (FEA) codes executed for transient load histories. Examples are provided to demonstrate the features of the methodology as implemented in the CARES/Life program.

Nemeth, Noel N.↗

NASA NTRS2004

Simulation of Foam Impact Effects on Components of the Space Shuttle Thermal Protection System

A series of three dimensional simulations has been performed to investigate analytically the effect of insulating foam impacts on ceramic tile and reinforced carbon-carbon components of the Space Shuttle thermal protection system. The simulations employed a hybrid particle-finite element method and a parallel code developed for use in spacecraft design applications. The conclusions suggested by the numerical study are in general consistent with experiment. The results emphasize the need for additional material testing work on the dynamic mechanical response of thermal protection system materials, and additional impact experiments for use in validating computational models of impact effects.

Fahrenthold, Eric P.↗

DOE OSTI2022

ADDITIVELY MANUFACTURED SURFACE HEAT TRANSFER ENHANCEMENTS FOR THE TRANSFORMATIONAL CHALLENGE REACTOR

The Transformational Challenge Reactor (TCR) is a high-temperature gas-cooled reactor design that uses additively manufactured fuel elements. TCR fuel elements have walls made of silicon carbide and are filled with tristructural-isotropic fuel particles. These fuel elements can have radically different shapes and integrated features than existing designs due to the reduced cost for complex structures in binder jet additive manufacturing. As such, binder jet additive manufacturing enables wall surface features to be embedded that can deliver superior heat transfer performance than smooth wall designs. In this work, the authors conducted a computational fluid dynamics study to evaluate selected wall features integrated into TCR fuel elements. Results show that surface features can outperform smooth wall designs; however, there are unique challenges for gas-cooled reactor core designs that have not been fully explored by previous research. For example, the rough surface finish and process variability of ceramics additive manufacturing make it challenging to predict surface roughness effects before fabrication. Additionally, the small hydraulic diameters of coolant channels in reactor cores make it difficult to engineer surface features that do not significantly increase the pressure drop. Engineers must carefully size surface features for heat transfer enhancement in additive fuel elements to operate above the base material's surface roughness effects and below the coolant channel size.

Weinmeister, Justin↗

NASA NTRS1997

TPS Materials for Planetary Exploration

This paper will review the current material options, and near term developments, for thermal protection systems (TPS) of future space craft involving atmospheric entry. TPS is a very important element in the design of these vehicles, and can have large impact on the project risk and cost. The new family of light weight ceramic ablators illustrated by SIRCA and PIC will be discussed, along with state-of-the-art ablators including SLA-561V, Avcoat-5026, carbon-phenolic, and carbon-carbon.

Rasky, Daniel J.↗

NASA NTRS2009

Multilayer Electroactive Polymer Composite Material Comprising Carbon Nanotubes

An electroactive material comprises multiple layers of electroactive composite with each layer having unique dielectric, electrical and mechanical properties that define an electromechanical operation thereof when affected by an external stimulus. For example, each layer can be (i) a 2-phase composite made from a polymer with polarizable moieties and an effective amount of carbon nanotubes incorporated in the polymer for a predetermined electromechanical operation, or (ii) a 3-phase composite having the elements of the 2-phase composite and further including a third component of micro-sized to nano-sized particles of an electroactive ceramic incorporated in the polymer matrix.

Ounaies, Zoubeida↗

NASA NTRS2011

Multilayer Electroactive Polymer Composite Material

Ounaies, Zoubeida↗

DOE OSTI2025

Microwave Debinding of Ceramics Produced by Additive Manufacturing

Microwave-assisted debinding offers an innovative approach to processing 3D-printed engineering ceramics. Ceramic parts produced with photopolymer-based additive manufacturing techniques require thermal debinding to remove polymers that bind ceramic particles during the printing process. Microwave-assisted debinding significantly reduces processing times and offers energy savings over conventional thermal treatments due to higher heating rates and more uniform heating. Finite-element modeling of the debinding process allows for the optimization and prediction of temperature distribution, stress development, and potential defects, leading to improved process control and material quality.

36 - MATERIALS SCIENCE↗

NASA NTRS2017

Environmental Barrier Coating Fracture, Fatigue and High-Heat-Flux Durability Modeling and Stochastic Progressive Damage Simulation

Advanced environmental barrier coatings will play an increasingly important role in future gas turbine engines because of their ability to protect emerging light-weight SiC/SiC ceramic matrix composite (CMC) engine components, further raising engine operating temperatures and performance. Because the environmental barrier coating systems are critical to the performance, reliability and durability of these hot-section ceramic engine components, a prime-reliant coating system along with established life design methodology are required for the hot-section ceramic component insertion into engine service. In this paper, we have first summarized some observations of high temperature, high-heat-flux environmental degradation and failure mechanisms of environmental barrier coating systems in laboratory simulated engine environment tests. In particular, the coating surface cracking morphologies and associated subsequent delamination mechanisms under the engine level high-heat-flux, combustion steam, and mechanical creep and fatigue loading conditions will be discussed. The EBC compostion and archtechture improvements based on advanced high heat flux environmental testing, and the modeling advances based on the integrated Finite Element Analysis Micromechanics Analysis Code/Ceramics Analysis and Reliability Evaluation of Structures (FEAMAC/CARES) program will also be highlighted. The stochastic progressive damage simulation successfully predicts mud flat damage pattern in EBCs on coated 3-D specimens, and a 2-D model of through-the-thickness cross-section. A 2-parameter Weibull distribution was assumed in characterizing the coating layer stochastic strength response and the formation of damage was therefore modeled. The damage initiation and coalescence into progressively smaller mudflat crack cells was demonstrated. A coating life prediction framework may be realized by examining the surface crack initiation and delamination propagation in conjunction with environmental degradation under high-heat-flux and environment load test conditions.

Mechanical creep and fatigue loading condition↗

NASA NTRS1986

Ultrasonic characterization of microstructure in powder metal alloy

The ultrasonic wave propagation characteristics were measured for IN-100, a powder metallurgy alloy used for aircraft engine components. This material was as a model system for testing the feasibility of characterizing the microstructure of a variety of inhomogeneous media including powder metals, ceramics, castings and components. The data were obtained for a frequency range from about 2 to 20 MHz and were statistically averaged over numerous volume elements of the samples. Micrographical examination provided size and number distributions for grain and pore structure. The results showed that the predominant source for the ultrasonic attenuation and backscatter was a dense (approx. 100/cubic mm) distribution of small micropores (approx. 10 micron radius). Two samples with different micropore densities were studied in detail to test the feasibility of calculating from observed microstructural parameters the frequency dependence of the microstructural backscatter in the regime for which the wavelength is much larger than the size of the individual scattering centers. Excellent agreement was found between predicted and observed values so as to demonstrate the feasibility of solving the forward problem. The results suggest a way towards the nondestructive detection and characterization of anomalous distributions of micropores when conventional ultrasonic imaging is difficult. The findings are potentially significant toward the application of the early detection of porosity during the materials fabrication process and after manufacturing of potential sites for stress induced void coalescence leading to crack initiation and subsequent failure.

Tittmann, B. R.↗

NASA NTRS2013

Laboratory Instruments Available to Support Space Station Researchers at Marshall Space Flight Center

A number of research instruments are available at NASA's Marshall Space Flight Center (MSFC) to support ISS researchers and their investigations. These modern analytical tools yield valuable and sometimes new informative resulting from sample characterization. Instruments include modern scanning electron microscopes equipped with field emission guns providing analytical capabilities that include angstron-level image resolution of dry, wet and biological samples. These microscopes are also equipped with silicon drift X-ray detectors (SDD) for fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations in crystalline alloys. Sample chambers admit large samples, provide variable pressures for wet samples, and quantitative analysis software to determine phase relations. Advances in solid-state electronics have also facilitated improvements for surface chemical analysis that are successfully employed to analyze metallic materials and alloys, ceramics, slags, and organic polymers. Another analytical capability at MSFC is a mganetic sector Secondary Ion Mass Spectroscopy (SIMS) that quantitatively determines and maps light elements such as hydrogen, lithium, and boron along with their isotopes, identifies and quantifies very low level impurities even at parts per billion (ppb) levels. Still other methods available at MSFC include X-ray photo-electron spectroscopy (XPS) that can determine oxidation states of elements as well as identify polymers and measure film thicknesses on coated materials, Scanning Auger electron spectroscopy (SAM) which combines surface sensitivity, spatial lateral resolution (approximately 20 nm), and depth profiling capabilities to describe elemental compositions in near surface regions and even the chemical state of analyzed atoms. Conventional Transmission Electron Microscope (TEM) for observing internal microstructures at very high magnifications and the Electron Probe Micro-analyzer (EPMA) for very precise microanalysis are available as needed by the researcher. Space Station researchers are invited to work with MSFC in analyzing their samples using these techniques.

Panda, Binayak↗

DOE OSTI2020

Quantifying leakage fields at ionic grain boundaries using off-axis electron holography

The electrical properties of interfaces in semiconductors and ionic conductors are immensely important in a wide range of applications. Electron holography is ideally suited for the direct measurement of the electrostatic potential of such interfaces. A key challenge with this approach is the contribution of the leakage field from the sample to the observed electron phase shift. This leakage field cannot be a priori independently determined and can cause an overestimation of the phase shift. In this work, we use finite element simulations to compute the three-dimensional electrostatic potential in the vicinity of an interface associated with a given interfacial charge density distribution. We then evaluate the predicted phase shift and demonstrate that the leakage field strongly affects the recovery of the projected interface potential. From the difference between the true potential and uncorrected, recovered potential, we propose a method to correct for this effect. We then demonstrate the application of this methodology to the analysis of experimental off-axis electron holography data acquired from the grain boundaries in lightly doped ceria.

36 MATERIALS SCIENCE↗