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At least 19 records

X-ray Micro-Tomography of Ablative Heat Shield Materials

X-ray micro-tomography is a non-destructive characterization technique that allows imaging of materials structures with voxel sizes in the micrometer range. This level of resolution makes the technique very attractive for imaging porous ablators used in hypersonic entry systems. Besides providing a high fidelity description of the material architecture, micro-tomography enables computations of bulk material properties and simulations of micro-scale phenomena. This presentation provides an overview of a collaborative effort between NASA Ames Research Center and Lawrence Berkeley National Laboratory, aimed at developing micro-tomography experiments and simulations for porous ablative materials. Measurements are carried using x-rays from the Advanced Light Source at Berkeley Lab on different classes of ablative materials used in NASA entry systems. Challenges, strengths and limitations of the technique for imaging materials such as lightweight carbon-phenolic systems and woven textiles are discussed. Computational tools developed to perform numerical simulations based on micro-tomography are described. These enable computations of material properties such as permeability, thermal and radiative conductivity, tortuosity and other parameters that are used in ablator response models. Finally, we present the design of environmental cells that enable imaging materials under simulated operational conditions, such as high temperature, mechanical loads and oxidizing atmospheres.Keywords: Micro-tomography, Porous media, Ablation

tomography

X-Ray Micro-Tomography Applied to Nasa's Materials Research: Heat Shields, Parachutes and Asteroids

X-ray micro-tomography is used to support the research on materials carried out at NASA Ames Research Center. The technique is applied to a variety of applications, including the ability to characterize heat shield materials for planetary entry, to study the Earth- impacting asteroids, and to improve broadcloths of spacecraft parachutes. From micro-tomography images, relevant morphological and transport properties are determined and validated against experimental data.

asteroids

Search for Fluid Inclusions in a Carbonaceous Chondrite Using a New X-Ray Micro-Tomography Technique Combined with FIB Sampling

Early solar system aqueous fluids are preserved in some H chondrites as aqueous fluid inclusions in halite (e.g., [1]). Although potential fluid inclusions are also expected in carbonaceous chondrites [2], they have not been surely confirmed. In order to search for these fluid inclusions, we have developped a new X-ray micro-tomography technique combined with FIB sampling and applied this techniqu to a carbanaceous chondrite. Experimental: A polished thin section of Sutter's Mill meteorite (CM) was observed with an optical microscope and FE-SEM (JEOL 7001F) for chosing mineral grains of carbonates (mainly calcite) and sulfides (FeS and ZnS) 20-50 microns in typical size, which may have aqueous fluid inclusions. Then, a "house" similar to a cube with a roof (20-30 microns in size) is sampled from the mineral grain by using FIB (FEI Quanta 200 3DS). Then, the house was atached to a thin W-needle by FIB and imaged by a SR-based imaging microtomography system with a Fresnel zone plate at beamline BL47XU, SPring-8, Japan. One sample was imaged at two X-ray energies, 7 and 8 keV, to identify mineral phases (dual-enegy microtomography: [3]). The size of voxel (pixel in 3D) was 50-80 nm, which gave the effective spatial resolution of approx. 200 nm. A terrestrial quartz sample with an aqueous fluid inclusion with a bubble was also examined as a test sample by the same method. Results and discussion: A fluid inclusion of 5-8 microns in quartz was clearly identified in a CT image. A bubble of approx. 4 microns was also identified as refraction contrast although the X-ray absorption difference between fluid and bubble is small. Volumes of the fluid and bubble were obtained from the 3D CT images. Fourteen grains of calcite, two grains of iron sulfide and one grain of (Zn,Fe)S were examined. Ten calcite, one iron sulfide and one (Zn,Fe)S grains have inclusions >1 micron in size (the maximum: approx. 5 microns). The shapes are spherical or irregular. Tiny inclusions (<1 micron) are also present in all the grains examined. These results show that mineral grains have more inclusions than expected from 2D observations. The X-ray absorption of the inclusions shows that they are not solid inclusions. No bubbles were observed inside, indicating that we cannot determine whether they are really aqueous fluids or merely voids. One calcite grain has an inclusion approx. 2 microns in size, which seems to have a bubble and a tiny solid daughter crystal inside (three-phase inclusion). As we know the exact 3D position of the inclusion, we will anlyze the inclusion by SIMS after freezing the sample as has been done for a halite sample [3]. The present technique is useful for finding small inclusions not only in carbonaceous chondrites but also for terrestrial materials.

Tsuchiyama, A.

Analysis of Fibrous Felts for Flexible Ablators Using Synchrotron Hard X-Ray Micro-Tomography

We analyzed the material properties of low-density felts that are used as substrates for new-generation flexible and conformal carbon/phenolic ablators, and compared them with those of a rigid carbon fiber preform that is used to manufacture rigid carbon/phenolic ablators. Micro-tomography measurements were obtained using synchrotron X-rays, allowing the characterization of the materials microstructure at the scale of the fibers. Using the tomography voxels as computational grids, we computed tortuosity and room temperature conductivity. In addition we performed micro-scale simulations of the oxidation of carbon fibers using a random walk model for oxygen diffusion and a probability law to model surface reactions.

Ablation

Investigation of the temperature-dependent failure processes in PVD Cr-coated ZIRLO nuclear fuel cladding using in situ X-ray micro-tomography imaging

In this work, an accident tolerant fuel cladding system with Cr coating deposited using physical vapour deposition (PVD) method onto commercial Optimized ZIRLO™ was studied. The cladding tubes were machined into C-rings and loaded to failure under compression with real-time synchrotron micro-X-ray computed tomography (XCT) imaging at room temperature (RT), 345 °C, 650 °C and 950 °C in argon (Ar) atmosphere. The mechanical behaviour and failure processes were found strongly temperature-dependent where the Cr coating showed brittle fracture at RT and 345 °C, ductile fracture at 650 °C and a reversion to brittle fracture at 950 °C. Nanoindentation measurements and scanning electron microscopy (SEM) imaging were conducted on the materials after high temperature testing. It was found that recrystallisation of the Cr coating occurred at elevated temperatures, which significantly affected its local properties hence the failure behaviour at different temperatures. This work represents the first in situ 3D XCT observation of progressive failure processes in PVD Cr-coated ZIRLO claddings up to 950 °C providing critical insights into its brittle-to-ductile transition (BDTT) behaviour and subsequent ductile-to-brittle reversion with the increase in temperature. Moreover, results are compared with other PVD Cr-coated Zircaloy materials from open literature; the influences of the coating microstructure and local properties on the failure stress/strain and fracture processes are discussed.

Yuan, Guanjie

From Tomography to Material Properties of Thermal Protection Systems

A NASA Ames Research Center (ARC) effort, under the Entry Systems Modeling (ESM) project, aims at developing micro-tomography (micro-CT) experiments and simulations for studying materials used in hypersonic entry systems. X-ray micro-tomography allows for non-destructive 3D imaging of a materials micro-structure at the sub-micron scale, providing fiber-scale representations of porous thermal protection systems (TPS) materials. The technique has also allowed for In-situ experiments that can resolve response phenomena under realistic environmental conditions such as high temperature, mechanical loads, and oxidizing atmospheres. Simulation tools have been developed at the NASA Ames Research Center to determine material properties and material response from the high-fidelity tomographic representations of the porous materials with the goal of informing macroscopic TPS response models and guiding future TPS design.

Tomography

Modeling the Relationship Between Porosity and Permeability During Oxidation of Ablative Materials

The ablative materials used in thermal protection systems (TPS) undergo oxidation during atmospheric entry which leads to an in-depth change in both permeability and porosity. These properties have a significant affect on heat transfer in a TPS during entry. X-ray micro-tomography has provided 3D images capturing the micro-structure of TPS materials. In this study, we use micro-tomography based simulations to create high-fidelity models relating permeability to porosity during oxidation of FiberForm, the carbon fiber preform of the Phenolic Impregnated Carbon Ablator (PICA) often used as a TPS material. The goal of this study is to inform full-scale models and reduce uncertainty in TPS modeling.

Ablativ

From Tomography to Material Properties of Thermal Protection Systems

The X-ray micro-tomography technique provides non-destructive characterizations of three-dimensional material micro-structures at spatial resolutions from the sub-micron to the centimeter scale. High quality micro-tomography images of NASA Thermal Protection System (TPS) materials are obtained using one of the brightest synchrotron X-ray sources available. Leveraging on NASA supercomputing capabilities, material properties and response are computed from tomography-data. This talk highlights the process and challenges of going from 3D images of actual material structures to simulations of properties and phenomena relevant to TPS material response, such as thermal conductivity, permeability, mass transport and high temperature reactions. The talk is addressed to a broad audience including scientists, engineers, researchers, educators, programmers, managers, and members of the media.

tomography

Root‐Pore Interactions, the Underestimated Driver for Rhizosphere Structure and Rhizosheath Development

Physical characteristics of rhizosphere and rhizosheath, that is, root-adhering soil, are crucial for plant performance. Yet, the drivers of the rhizosphere's structural properties and their relationships with rhizosheath development remain unclear. We used X-ray computed micro-tomography (i) to explore two drivers of rhizosphere porosity: root-induced changes vs. preferential root growth into soil with certain pore characteristics and (ii) to estimate their contributions to rhizosphere macroporosity gradients and rhizosheath formation. Rhizosheath development was assessed in relation to rhizosphere macroporosity and rhizodeposition after ¹⁴C labeling. Our results confirmed that both root-induced changes and growth preferences shape rhizosphere structure, with their relative significance depending on the inherent macropore availability. In intact soils, growth preferences were the dominant factor, while in sieved soils the root-induced changes became equally important. Rhizosheath formation was associated with roots compacting their surrounding and releasing carbon. However, no correlation was found between rhizosheath formation and the actual rhizosphere, that is, the volume of soil adjacent to the roots. The study offers new process-level understanding of rhizosphere porosity gradients, while emphasizing caution in interpreting root growth data from sieved soil studies. Similarly, traditional destructively sampled rhizosheath may not fully capture the true characteristics of the actual rhizosphere, underscoring importance of intact-soil analyses.

macroporosity gradients

Soil carbon accrual and biopore formation across a plant diversity gradient

Plant diversity promotes soil organic carbon (SOC) gains through intricate changes in root-soil interactions and their subsequent influence on soil physical and biological processes. We assessed SOC and pore characteristics of soils under a range of switchgrass-based plant systems 12 years after their establishment. The systems represented a gradient of plant diversity with species richness ranging from 1 to 30 species. We focused on soil biopores as indicators of the legacy of root activity and explored biopore relationships with SOC accumulation. Biopores were measured using X-ray computed micro-tomography. Plant functional richness explained 29 % of bioporosity and 36 % of SOC variation, while bioporosity itself explained 36 % of the variation in SOC. The most diverse plant system (30 species) had the highest SOC, while long-term bare soil fallow and monoculture switchgrass had the lowest. Of particular note was a 2-species mixture of switchgrass (Panicum virgatum L.) and ryegrass (Elymus canadensis), which exhibited the highest bioporosity and achieved SOC levels comparable to those of the systems with 6 and 10 plant species, and were inferior only to the system with 30 species. We conclude that plant diversity may enhance SOC through biopore-mediated mechanisms and suggest a potential for identifying specific plant combinations that may be particularly efficient for fostering biopore formation and, subsequently, SOC sequestration.

Kim, Kyungmin [Seoul National Univ. (Korea, Republ

Oxygen and Magnesium Isotopic Compositions of Asteroidal Materials Returned from Itokawa by the Hayabusa Mission

The Hayabusa spacecraft made two touchdowns on the surface of Asteroid 25143 Itokawa on November 20th and 26th, 2005. The Asteroid 25143 Itokawa is classified as an S-type asteroid and inferred to consist of materials similar to ordinary chondrites or primitive achondrites [1]. Near-infrared spectroscopy by the Hayabusa spacecraft proposed that the surface of this body has an olivine-rich mineral assemblage potentially similar to that of LL5 or LL6 chondrites with different degrees of space weathering [2]. The spacecraft made the reentry into the Earth s atmosphere on June 12th, 2010 and the sample capsule was successfully recovered in Australia on June 13th, 2010. Although the sample collection processes on the Itokawa surface had not been made by the designed operations, more than 1,500 grains were identified as rocky particles in the sample curation facility of JAXA, and most of them were judged to be of extraterrestrial origin, and definitely from Asteroid Itokawa on November 17th, 2010 [3]. Although their sizes are mostly less than 10 microns, some larger grains of about 100 microns or larger were also included. The mineral assembly is olivine, pyroxene, plagioclase, iron sulfide and iron metal. The mean mineral compositions are consistent with the results of near-infrared spectroscopy from Hayabusa spacecraft [2], but the variations suggest that the petrologic type may be smaller than the spectroscopic results. Several tens of grains of relatively large sizes among the 1,500 grains will be selected by the Hayabusa sample curation team for preliminary examination [4]. Each grain will be subjected to one set of preliminary examinations, i.e., micro-tomography, XRD, XRF, TEM, SEM, EPMA and SIMS in this sequence. The preliminary examination will start from the last week of January 2011. Therefore, samples for isotope analyses in this study will start from the last week of February 2011. By the time of the LPSC meeting we will have measured the oxygen and magnesium isotopic composition of several grains. We will present the first results from the isotope analyses that will have been performed.

Yurimoto, H

Investigation of the High-Energy Oxidation of FiberForm from DSMC Analysis of Molecular Beam Experiments

A collaborative effort between the University of Illinois at Urbana-Champaign (UIUC), NASA Ames Research Center (ARC) and Montana State University (MSU) succeeded at developing a new finite-rate carbon oxidation model from molecular beam scattering experiments on vitreous carbon (VC). We now aim to use the direct simulation Monte Carlo (DSMC) code SPARTA to apply the model to each fiber of the porous fibrous Thermal Protection Systems (TPS) material FiberForm (FF). The detailed micro-structure of FF was obtained from X-ray micro-tomography and then used in DSMC. Both experiments and simulations show that the CO/O products ratio increased at all temperatures from VC to FF. We postulate this is due to the larger number of collisions an O atom encounters inside the porous FF material compared to the flat surface of VC. For the simulations, we particularly focused on the lowest and highest temperatures studied experimentally, 1023 K and 1823 K, and found good agreement between the finite-rate DSMC simulations and experiments.

Oxidation

Tortuosity Computations of Porous Materials using the Direct Simulation Monte Carlo

Low-density carbon fiber preforms, used as thermal protection systems (TPS) materials for planetary entry systems, have permeable, highly porous microstructures consisting of interlaced fibers. Internal gas transport in TPS is important in modeling the penetration of hot boundary-layer gases and the in-depth transport of pyrolysis and ablation products. The gas effective diffusion coefficient of a porous material must be known before the gas transport can be modeled in material response solvers; however, there are very little available data for rigid fibrous insulators used in heritage TPS.The tortuosity factor, which reflects the efficiency of the percolation paths, can be computed from the effective diffusion coefficient of a gas inside a porous material and is based on the micro-structure of the material. It is well known, that the tortuosity factor is a strong function of the Knudsen number. Due to the small characteristic scales of porous media used in TPS applications (typical pore size of the order of 50 micron), the transport of gases can occur in the rarefied and transitional regimes, at Knudsen numbers above 1. A proper way to model the gas dynamics at these conditions consists in solving the Boltzmann equation using particle-based methods that account for movement and collisions of atoms and molecules.In this work we adopt, for the first time, the Direct Simulation Monte Carlo (DSMC) method to compute the tortuosity factor of fibrous media in the rarefied regime. To enable realistic simulations of the actual transport of gases in the porous medium, digitized computational grids are obtained from X-ray micro-tomography imaging of real TPS materials. The SPARTA DSMC solver is used for simulations. Effective diffusion coefficients and tortuosity factors are obtained by computing the mean-square displacement of diffusing particles.We first apply the method to compute the tortuosity factors as a function of the Knudsen number for computationally designed materials such as random cylindrical fibers and packed bed of spheres with prescribed porosity. Results are compared to literature values obtained using random walk methods in the rarefied and transitional regime and a finite-volume method for the continuum regime. We then compute tortuosity factors for a real carbon fiber material with a transverse isotropic structure (FiberForm), quantifying differences between through-thickness and in-plain tortuosities at various Knudsen regimes.

Tortuosity

Improved damage tolerance of SiC-based nuclear fuel cladding with novel multi-layered SiC coating design at 1200 °C

Continuous SiC fibre reinforced SiC matrix composites (SiC f -SiC m ) with monolithic SiC outer coatings are considered as a damage-tolerant cladding design for loss of coolant accident (LOCA) conditions in light water reactors. However, monolithic SiC coatings are brittle and prone to catastrophic failure. In this study, a SiC f -SiC m cladding with a novel multi-layer SiC outer coating (11 sub-layers, ∼260 µm in total thickness) was investigated under C-ring compression at room temperature and 1200 °C in argon environment. Real-time synchrotron X-ray computed tomography (XCT) was employed to capture crack initiation and propagation processes. Compared to conventional monolithic SiC outer coatings, the multi-layer coating structure facilitated crack deflection and bifurcation enhancing its damage tolerance at both temperatures. Despite pre-existing surface cracks, claddings exhibited stable mechanical-performance at both temperatures. These initial cracks did not critically affect the failure processes as they were not aligned with the maximum stress direction. Furthermore, the microstructure, distribution of residual stresses, and local properties of individual components in the material were thoroughly characterized, and compared with open literature on conventional claddings with monolithic outer coatings. These results provide new insights into the failure mechanisms of multi-layer SiC coatings and offer guidance for the future design of accident-tolerant nuclear fuel claddings.

36 - MATERIALS SCIENCE

Belowground plant carbon and nitrogen exchange: plant-derived carbon inputs and pore structure formation

Belowground plant transfer of carbon (C) and nitrogen (N) can benefit soil ecosystems, increasing soil C gains and plant N availability, while improving soil pore structure. We explored such transfers among three plant species of North American prairie, where C and N were transferred from a grass (Panicum virgatum L., switchgrass (Sgrass)) to either a legume (Lespedeza capitata Michx., bush clover (Bclover)), a forb (Rudbeckia hirta L., black-eyed Susan (BSforb)), or a mixture of the two. The plants were grown either with/out direct root contact, thus allowing assessment of the relative contributions of fungal- and root-based transfer pathways. The Sgrass was labeled with 13 C and 15 N, and C and N transfers were assessed by measuring isotope enrichment of roots and aboveground biomass of neighboring plants. Soil inputs of plant-derived C and N were assessed by isotope analyses of the rhizosphere soil. X-ray computed tomography was used for pore structure analyses. Carbon transfer was much higher in the presence of direct/close root contact between source and recipient plants, yet N transfers appeared to be mainly fungal driven. Here, while C and N were readily transferred from Sgrass to other Sgrass and Bclover neighbors, transfers to BSforb were negligible. However, in a three species system, the presence of the legume enhanced C and N transfers to BSforb, suggesting non-additive influences of diverse plant community composition. The more plant-derived C and N was found in the rhizosphere of recipient plants, the greater C and N transfers through roots. Greater C and N transfers were associated with increases in 8–30 μm diameter pores and decreases in >150 μm pores. Summarily, diverse plant communities, especially those with legumes, increase C and N transfers, which then benefit soil C inputs and its protection via changes in pore structure.

13 CO 2 pulse labeling

Thermo-Poro-Mechanical Modeling of RTV Intumescence

Room temperature vulcanizing (RTV) silicone is a high-temperature adhesive used as a gap-filler between heatshield tiles in numerous entry missions. Its propensity to intumesce, or swell upon exposure to heat, is a well-known effect that needs to be carefully quantified during design. At tile interfaces of charring ablators, intumescence, combined with differential recession, could cause the gap filler to protrude past the ablator outer mold line, forming a “fence”. Fencing can in turn cause transition to turbulence of the flow wetting the heat shield, leading to augmented surface heating. Recent experiments conducted at the Plasmatron X facility, the high enthalpy wind tunnel of the Center for Hypersonics and Entry Systems Studies, have shown prominent fencing of RTV gap fillers in PICA, under both nitrogen and air plasmas. Similar observations are well known in the arcjet literature. Further experiments under controlled environment, performed using in situ X-ray micro-computed tomography (micro-CT) at the Advanced Light Source (ALS), have shown heating rate-dependent swelling and shrinkage of RTV during pyrolysis. To simulate RTV intumescence, a novel model was introduced in the Porous Materials Analysis Toolbox based on OpenFOAM, PATO, to account for pore-pressure buildup within both closed- and open-pores. The governing equation for the thermo-poro-mechanical response were developed, assuming linear elasticity for the charring silicone. A new multi-pyrolysis model that tracks non-monotonic advancement of material properties with pyrolysis was proposed. This model addresses the limitations of state-of-the-art ablator models to capture the different stages of thermal degradation and coupled thermomechanics. Swelling of RTV was simulated using the new thermo-poro-mechanical model and compared against in situ micro-CT data. Results showed good agreement in intumescence height and temperature profiles at all heating rates, indicating that the key factor contributing to RTV swelling is the internal pressure build-up within closed- and open-pores. As RTV is cured into a soft (rubbery) compound with low-porosity and permeability, initial temperature increase and pyrolysis gas production cause a significant increase of internal pressure, causing a pronounced volume growth. As thermal degradation progresses, rigidization of the silicone occurs due to char hardening which counteract volume shrinkage after gas pressure relief. Overall, our model shows that accounting for changes in properties such porosity, permeability and key thermomechanical coefficients is crucial for capturing the RTV volume change during ablation and enable a predictive capability for heatshield tile interface response. A plan for future calibration of thermomechanical properties evolution during degradation is discussed, as a key next step to close the new model.

RTV