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At least 469 records · Page 26

Fused silica reflecting heat shields for outer planet entry probes

The development of slip-cast fused silica is discussed as a heat shield designed to meet the needs of outer-planet entry probes. The distinguishing feature of silica is its ability to reflect the radiation imposed by planetary-entry environments. This reflectivity is particularly sensitive to degradation by the presence of trace amounts of contaminants introduced by the starting materials or by processing. The microstructure of a silica configuration also significantly influences the reflectivity and other thermomechanical properties. The processing techniques attendant on controlling microstructure while maintaining purity are discussed. The selection of a starting material of essential purity precludes the use of purified natural quartz and requires the use of synthetic fused silica. The silica is characterized in a limited combined heating test environment. The surface mass loss is controlled by liquid runoff from a relatively low-temperature melt layer; the reflectance is basically maintained and the material achieves a surprisingly high heat of ablation.

Congdon, W. M.↗

NanoSIMS Sheds Light on the Origin and Significance of Early Archean Organic Microstructures from the Pilbara of Australia

NanoSIMS was used to characterize sub-micron scale morphology and elemental composition (C, N, S, Si, O) of organic microstructures in Early Archean (3 - 3.4 Ga) charts from the Pilbara of Western Australia. Three categories of structures were analyzed: small spheroids in clusters; spindle-shaped remains; and large spheroids. All are relatively poorly preserved and occur within the chert matrix of the samples. Carbonaceous material in a secondary hydrothermal vein also was analyzed, as an example of non-indigenous organic matter. Comparisons were made of NanoSIMS characteristics of the Archean samples and those from well-preserved, biogenic microfossils in the 0.8 Ga Bitter Springs Formation. The comparisons show that the Pilbara microstructures are generally distinct from material in the hydrothermal vein but similar in morphology and elemental composition to the Bitter Springs microfossils. In addition, the Pilbara structures exhibit a spatial relationship to silicon and oxygen that seemingly reflects silica nucleation on organic surfaces; this argues that the organic frameworks of the Archean structures were present in the sediment during crystallization of the silica matrix. The structures are thus interpreted as being indigenous to the enclosing sediment. While these results are suggestive of Early Archean biogenicity and are consistent with a growing body of data suggesting that life on Earth was well established by 3 to 3.4 Ga, work is continuing to determine the N/C and 13C ratios of individual forms, and this should provide additional insight into the derivation and significance of these ancient organic remains.

Oehler, Dorothy Z.↗

Development of silicon nitride of improved toughness

The application of reaction sintered Si2N4 energy absorbing surface layers to hot-pressed Si3N4 was investigated. The surface layer was formed by in-place nitridation of silicon powder. It was found that reaction sintered Si3N4 layers of 1 mm thickness, fabricated from either -100, +200, -200, or -325 mesh Si powder and nitrided in 96% N2/4% H2 so that approximately 20-25 vol % unnitrided Si remained in the layer, resulted in a sevenfold increase in ballistic impact resistance of a 0.64 cm thick hot-pressed SI3N4 substrate from RT 1370 C. Both NC-132 SI3N4, with MgO additive, and NCX-34 Si3N4, with Y2O3 additive, were evaluated as substrate material. The finer grain size -200 and -325 mesh nitrided Si layers were for their smoothness and relatively high density. It was found that nitriding in N2/H2 mixtures, rather than pure N2, resulted in a microstructure that did not substantially degrade the strength of the hot-pressed Si3N4 substrate. Thermal cycling tests on the RSSN/HPSN combinations from 200 C to 1370 C for 75 cycles in air did not degrade the impact resistance nor the interfacial bonding, although a large amount of internal silica formation occurred within the RSSN layer. Mach 0.8, 5 hr, hot gas erosion tests showed no surface recession of RSSN layers at 1200 C and slight surface recession at 1370 C.

Brennan, J. J.↗

Rapid solidification of highly undercooled liquids

Melt undercooling is considered as a fundamental processing parameter for powders and for melt-spun and surface-melted samples. With reference to experimental results for Mn, Al, Al-Be, Al-Fe, and InSb-Sb powders, it is shown that the undercooling behavior in droplets is influenced by powder size, coating, melt superheat, and cooling rate. Droplet sample microstructures can be compared directly with those of rapidly quenched powders to establish the application of laboratory-scale studies to large-scale processing.

Perepezko, J. H.↗

Microstructural and strength stability of CVD SiC fibers in argon environment

The room temperature tensile strength and microstructure of three types of commercially available chemically vapor deposited silicon carbide fibers were measured after 1, 10, and 100 hour heat treatments under argon pressures of 0.1 to 310 MPa at temperatures to 2100 C. Two types of fiber had carbon-rich surface coatings and the other contained no coating. All three fiber types showed strength degradation beyond 1400 C. Time and temperature of exposure had greater influence on strength degradation than argon pressure. Recrystallization and growth of near stoichiometric SiC grains appears to be the dominant mechanism for the strength degradation.

Bhatt, Ramakrishna T.↗

Microstructural and strength stability of CVD SiC fibers in argon environments

The room temperature tensile strength and microstructure of three types of commercially available chemically vapor deposited silicon carbide fibers were measured after 1, 10, and 100 hour heat treatments under argon pressures of 0.1 to 310 MPa at temperatures to 2100 C. Two types of fiber had carbon-rich surface coatings and the other contained no coating. All three fiber types showed strength degradation beyond 1400 C. Time and temperature of exposure had greater influence on strength degradation than argon pressure. Recrystallization and growth of near stoichiometric SiC grains appears to be the dominant mechanism for the strength degradation.

Bhatt, Ramakrishna T.↗

Investigation of Effects of Material Architecture on the Elastic Response of a Woven Ceramic Matrix Composite

To develop methods for quantifying the effects of the microstructural variations of woven ceramic matrix composites on the effective properties and response of the material, a research program has been undertaken which is described in this paper. In order to characterize and quantify the variations in the microstructure of a five harness satin weave, CVI SiC/SiC, composite material, specimens were serially sectioned and polished to capture images that detailed the fiber tows, matrix, and porosity. Open source quantitative image analysis tools were then used to isolate the constituents and collect relevant statistics such as within ply tow spacing. This information was then used to build two dimensional finite element models that approximated the observed section geometry. With the aid of geometrical models generated by the microstructural characterization process, finite element models were generated and analyses were performed to quantify the effects of the microstructure and its variation on the effective stiffness and areas of stress concentration of the material. The results indicated that the geometry and distribution of the porosity appear to have significant effects on the through-thickness modulus. Similarly, stress concentrations on the outer surface of the composite appear to correlate to regions where the transverse tows are separated by a critical amount.

Goldberg, Robert K.↗

Reactions of SiC with H2/H2O/Ar mixtures at 1300 C

Thermochemical modeling anticipates the existence of three reaction regions for the case of a sintered alpha-SiC with 5 percent H2/H2O/Ar at 1300 C, depending on the initial water vapor or, equivalently, oxygen, content of the gas stream. While a high oxygen content leads to SiC-protecting SiO2 surface film formation and limits consumption of the SiC through passive oxidation, intermediate oxygen contents lead to SiO and CO formation and rapid SiC consumption. In this intermediate region, reaction rates appear to be controlled by H2O gas-phase transport to the sample; reacted microstructures exhibit extensive grain-boundary attack in this region. Very low oxygen content is predicted to selectively remove carbon, with free silicon formation.

Jacobson, Nathan S.↗

Axial-torsional fatigue - A study of tubular specimen thickness effects

Experiments were carried out at room temperature on AISI type 316 stainless steel to determine the effect of wall thickness on the cyclic deformation behavior and fatigue life of thin-wall tubular axial-torsional fatigue specimens. The experimental variables examined included the depth of the surface work-hardened layer produced in specimen machining, and the effects of strain range and axial-torsional strain phasing. Tubular fatigue specimens had wall thicknesses of 1.5, 2.0, and 2.5 mm. One as-fabricated specimen from each wall thickness was sectioned for microstructural examination and microhardness measurement. A specimen of each wall thickness was tested in axial-torsional fatigue experiments for each of the three conditions: high strain range in-phase, low strain range in-phase, and low strain range out-of-phase. The machining-induced work-hardened zone, as a percentage of the gage section material, was found to have a minimal effect on both deformation behavior and fatigue life. Out-of-phase fatigue tests displayed shorter fatigue lives and more cyclic hardening than in-phase tests.

Bonacuse, Peter J.↗

Biologically-Derived Photonic Materials for Thermal Protection Systems

Space vehicles entering a planetary atmosphere at high velocity can be subject to substantial radiative heating from the shock layer in addition to the convective heating caused by the flow of hot gas past the vehicle surface. The radiative component can be very high but of a short duration. Approaches to combat this effect include investigation of various materials to reflect the radiation. Photonic materials can be used to reflect radiation. The wavelengths reflected depend on the length scale of the ordered microstructure. Fabricating photonic structures, such as layers, can be time consuming and expensive. We have used a biologically-derived material as the template for forming a high temperature photonic material that could be incorporated into a heatshield thermal protection material.

photonics↗

Aqueous alteration of Cb-type asteroid Ryugu

The samples from the asteroid Ryugu, which returned to Earth in the winter of 2020 [1], were stored under pure Nitrogen conditions at the Extraterrestrial Materials Curation Center of ISAS. After basic description [2-3], they were distributed to six initial analysis teams in Japan in June 2021. The initial analysis "Stone" team, which was responsible for the analysis of coarse particles (>1 mm in size), consisted of about 150 scientists from Japan and abroad, and conducted a series of analyses We analyzed sixteen coarse Ryugu particles 1 ~ 8 mm in size: six from the 1st touch-down site and ten from the 2nd touch-down site. Individual coarse samples were cut by Xe-FIB or wire-saw to expose particular objects or textures to be exposed on the surface based on 3D structure and element distribution obtained by synchrotron X-ray CT analysis and XRF analysis, respectively. FE-SEM/EDS and FE-EPMA/WDS analysis were made on all polished sections. TEM observation of many FIB sections was made to see microstructures and to compare with carbonaceous chondrites. Many other analyses were carried out to characterize mineralogical and compositional properties and summary of the analysis procedures is described in [4]. X-ray CT analysis showed that all sixteen Ryugu particles are composed of fine-grained material, with no chondrules and CAIs larger than 100 μm in size. FE-EPMA observation showed that Ryugu samples are breccias, consisting of many small rock fragments of different compositions, lithologies, and histories. The most common lithology includes Mg-rich saponite and serpentine, dolomite, magnesite, hydroxyapatite, pyrrhotite, and magnetite as main constituents. The mineralogy of this major lithology supports the classification of Ryugu samples as CI chondrites, which experienced extensive aqueous alteration in Ryugu’s parent asteroid. Based on the obtained mineralogical properties, we performed chemical modeling of aqueous alteration of Ryugu’s parent asteroid [5]. Numerical simulations [6-8] to reproduce thermal history and impact-induced destruction of the Ryugu’s parent asteroid were also carried out using mineralogical and physical properties of the Ryugu samples. In the talk, I would like to explain the conditions of aqueous alteration occurred in the parent asteroid of Ryugu in order to show how the water in the asteroid changed the mineralogy and chemistry of the nebular dust.

T. Nakamura↗

Measuring the Density, Viscosity, and Surface Tension of Molten Titanates Using Electrostatic Levitation in Microgravity

Rare earth and barium titanates are useful as ferroelectric, dielectric, and optical materials. Measurements of their thermophysical properties in the liquid state can help guide melt processing technologies for their manufacture and advance understanding of fragile liquids' behavior and glass formation. Here, we report the density, thermal expansion, viscosity, and surface tension of molten BaTiNsub>2 O 5 , BaTi 4 O 9 , and 83TiO 2 -17RE 2 O 3 (RE = La or Nd). Measurements were made using electrostatic levitation and droplet oscillation techniques in microgravity, which provide access to quiescent liquid droplets and deep supercooling of 510–815 K below the equilibrium melting points. Densities were measured over 900–2400 K. Viscosities were similar for all four compositions, increasing from ∼10 mPa s near 2100 K to ∼30 mPa s near 1750 K. Surface tensions were 450–490 dyn cm −1 for the rare earth titanates and 383–395 dyn cm−1 for the barium titanates; surface tensions of all compositions had small or negligible temperature dependence over 1700–2200 K. For solids recovered after melt quenching, x-ray microtomography revealed the fracture mechanics in crystalline products and minimal internal porosity in glass products, likely arising from entrapped gas bubbles. Internal microstructures were generally similar for products processed either in microgravity or in a terrestrial aerodynamic levitator.

Stephen K Wilke↗

Microstructural investigations of light-emitting porous Si layers

The structural and morphological characteristics of visible-light-emitting porous Si layers produced by anodic and stain etching of single-crystal Si substrates are compared using transmission electron microscopy and atomic force microscopy (AFM). AFM of conventionally anodized, laterally anodized and stain-etched Si layers show that the layers have a fractal-type surface morphology. The anodized layers are rougher than the stain-etched films. At higher magnification 10 nm sized hillocks are visible on the surface. Transmission electron diffraction patterns indicate an amorphous structure with no evidence for the presence of crystalline Si in the near-surface regions of the porous Si layers.

George, T.↗

Ferromagnetic phase-mass equivalence and lunar sample magnetic remanence

Man-made alloy spheres simulating the compositions of particles found in the lunar soil and weighting approximately 10 mg are shown to be equivalent, insofar as remanence intensity and demagnetization stability are concerned, to more than about 10 billion submicrometer spherical iron particles. The large particles not only contain large stable magnetic remanence, but when the polished surfaces of these particles are etched and carefully studied, they provide useful petrogenetic information, imply the mechanism of magnetization, the time-temperature history, and outline the format for possible paleointensity analysis. The intensity and stability of the remanence in these large spheres is related to the microstructure developed during rapid cooling.

Wasilewski, P. J.↗

Axial-torsional fatigue: A study of tubular specimen thickness effects

A room-temperature experimental program was conducted on AISI type 316 stainless steel to determine the effect of wall thickness on the cyclic deformation behavior and fatigue life of thin-wall, tubular, axial-torsional fatigue specimens. The following experimental variables were examined in this study: the depth of the surface work-hardened layer produced in specimen machining, and the effects of strain range and axial-torsional strain phasing. Tubular fatigue specimens were fabricated with wall thicknesses of 1.5, 2.0, and 2.5 mm. One as-fabricated specimen from each wall thickness was sectioned for microstructural examination and microhardness measurement. A specimen of each wall thickness was tested at each of three conditions - high strain range in-phase, low strain range in-phase, and low strain range out-of-phase - for a total of nine axial-torsional fatigue experiments. The machining-induced work-hardened zone, as a percentage of the gage section material, was found to have a minimal effect on both deformation behavior and fatigue life. Also, little or no variation in fatigue life or deformation behavior as a function of wall thickness was observed. Out-of-phase fatigue tests displayed shorter fatigue lives and more cyclic hardening than in-phase tests.

Bonacuse, Peter J.↗

The Smallest Lunar Grains: Analytical TEM Characterization of the Sub-micron Size Fraction of a Mare Soil

The chemical composition, mineralogical type, and morphology of lunar regolith grains changes considerably with decreasing size, and below the approx.25 m size range the correlation between these parameters and remotely-sensed lunar surface properties connected to space weathering increases significantly. Although trends for these parameters across grain size intervals greater than 20 m are now well established, the 0 to 20 m size interval remains relatively un-subdivided with respect to variations in grain modal composition, chemistry and microstructure. Of particular interest in this size range are grains in the approximate < 1 m diameter class, whose fundamental properties are now the focus of lunar research pertaining to electrostatic grain transport, dusty plasmas, and lunar dust effects on crew health and exploration systems. In this study we have used analytical transmission electron microscopy (TEM) to characterize the mineralogy, microstructure and major element composition of grains below the 1 m size threshold in lunar soil 10084.

Thompson, M.↗

Material Characterization and Modeling of Room Temperature Vulcanizing Silicone

Room Temperature Vulcanizing silicone (RTV) is a high-temperature adhesive that has successfully been used as a gap-filler between Thermal Protection System (TPS) tiles for heatshields on numerous missions. It is also used to bond instrumentation plugs such as temperature and pressure sensors into the heatshields. While RTV has been traditionally assumed to be a non-porous and non-ablating material, numerous experiments have shown that RTV pyrolyzes and becomes highly porous as it is heated. Heating RTV has also shown swelling, or intumescence, which can pose unique problems that lead to roughness induced boundary-layer transition, surface oxide formation and contamination of heat shield sensors. Therefore, it is crucial to understand and model the intumescence phenomenon of RTV. As data for RTV material properties is limited, the first step in modeling RTV is to collect material properties such as pyrolysis mass-loss, microstructure change, virgin and char porosity, etc. which was performed in our initial study. Additionally, thermomechanical properties such as Young’s modulus and Poisson ratio are required for modeling the intumescence of RTV, which were taken from literature and the coefficient of thermal expansion was collected using in-situ heating and Micro Computed Tomography (µ-CT) in previous studies. Finally, numerous other properties such as pyrolysis gas properties, virgin and char thermal conductivity and specific heat were compiled from previous experiments and literature into a material database that can be used for simulations. In Porous Material Analysis Toolbox based on OpenFOAM (PATO) [4], structural mechanics coupled with material response was used for simulating the intumescence of RTV as it is heated. However, since the permeability of the material is very low, the pyrolysis gas creates an internal pressure build-up as the material is being heated, significantly contributing to the deformation of the material. To correctly characterize this phenomenon, additional physics models were implemented into PATO's stress analysis solver, and results were compared with RTV dilatometry test data as a preliminary verification case. Future work will include experiments of RTV at the Plasmatron X facility and the in-situ heating cell with µ-CT, and improvement of simulation tools to more accurately model RTV intumescence.

TPS↗

Material Properties and Modeling of Room Temperature Vulcanizing Silicone

Room Temperature Vulcanizing silicone (RTV) is a high-temperature adhesive that has successfully been used as a gap-filler between Thermal Protection System (TPS) tiles for heatshields on numerous missions. It is also used to bond instrumentation plugs such as temperature and pressure sensors into the heatshields. While RTV has been traditionally assumed to be a non-porous and non-ablating material, numerous experiments have shown that RTV pyrolyzes and becomes highly porous as it is heated. Heating RTV has also shown swelling, or intumescence, which can pose unique problems that lead to roughness induced boundary-layer transition, surface oxide formation and contamination of heat shield sensors. Therefore, it is crucial to understand and model the intumescence phenomenon of RTV. As data for RTV material properties is limited, the first step in modeling RTV is to collect material properties such as pyrolysis mass-loss, microstructure change, virgin and char porosity, etc. which was performed in our initial study. Additionally, thermomechanical properties such as Young’s modulus and Poisson ratio are required for modeling the intumescence of RTV, which were taken from literature and the coefficient of thermal expansion was collected using in-situ heating and Micro Computed Tomography (µ-CT) in previous studies. Finally, numerous other properties such as pyrolysis gas properties, virgin and char thermal conductivity and specific heat were compiled from previous experiments and literature into a material database that can be used for simulations. In Porous Material Analysis Toolbox based on OpenFOAM (PATO) [4], structural mechanics coupled with material response was used for simulating the intumescence of RTV as it is heated. However, since the permeability of the material is very low, the pyrolysis gas creates an internal pressure build-up as the material is being heated, significantly contributing to the deformation of the material. To correctly characterize this phenomenon, additional physics models were implemented into PATO's stress analysis solver, and results were compared with RTV dilatometry test data as a preliminary verification case. Future work will include experiments of RTV at the Plasmatron X facility and the in-situ heating cell with µ-CT, and improvement of simulation tools to more accurately model RTV intumescence.

PATO↗