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NASA NTRS1984

Bubble formation in oxide scales on SiC

The oxidation of alpha-SiC single crystals and sintered alphaand beta-SiC polycrystals has been investigated at elevated temperatures. Bubble formation is commonly observed in oxide scales on polycrystalline SiC, but is rarely found on single-crystal scales; bubbles result from the preferential oxidation of C inclusions, which are abundant in SiC polycrystals. The absence of bubbles on single crystals, in fact, implies that diffusion of the gaseous species formed on oxidation, CO (or possibly SiO), controls the rate of oxidation of SiC.

Mieskowski, D. M.↗

NASA NTRS2002

Knowledge of Pest Resistance in SiC/BN/SiC Composites Improved

Ceramic-matrix composites (CMC's) consisting of a silicon carbide matrix reinforced with boron-nitride- (BN-) coated silicon carbide (SiC) fibers are strong contenders for commercial and aerospace applications (in particular, the hot sections of high-performance turbine engines in advanced aircraft and generators). They have very good mechanical properties below approximately 600 C and above approximately 1000 C. Between those temperatures, however, the BN coating oxidizes easily, and the oxidation of the SiC matrix is too sluggish to seal off the composite with a protective layer of silica. In that temperature interval, the preferential oxidation of the BN weakens and embrittles the composite. That phenomenon, referred to as "pest" degradation, is the focus of this work, which aims to identify the causes of and remedies for pesting. Previous work established that pesting in Hi-Nicalon (Nippon Carbon Co., Ltd., Japan)/SiC composites was caused by a layer of free carbon that undermined the oxidation resistance of the BN. New work suggests that composites containing a source of carbon are prone to severe pesting and that those that are free of elemental carbon are resistant pesting. Pest resistance was assessed by exposing machined samples for 100 to 150 hr in an atmospheric burner rig at 600 to 1100 C, followed by a tensile fracture test to measure residual mechanical properties and by characterization of the interphase microstructure. Whether the elemental carbon came from intrinsic or extrinsic sources, its presence induced the tensile strength to drop by over 50 percent in the burner rig, with an even more severe loss of fracture strain. A likely mechanism by which burnoff of the carbon layer exposes the BN to accelerated flank attack by ambient oxidants is shown. The BN is replaced with borosilicates that attack the fiber, and ultimately with silica that embrittles the composites by rigidly bonding components. Thus, the study has shown that pesting can be prevented in SiC/BN/SiC, or at least reduced, by simply excluding free carbon. These studies continue, and plans for future work include investigating the role that carbon may play elsewhere in the interphase region.

Thomas-Ogbuji, Linus U.↗

NASA NTRS2001

Delayed Alumina Scale Spallation on Rene'n5+y: Moisture Effects and Acoustic Emission

The single crystal superalloy Rene'N5 (with or without Y-doping and hydrogen annealing) was cyclically oxidized at 1150 C for 1000 hours. After considerable scale growth (>= 500 hours), even the adherent alumina scales formed on Y-doped samples exhibited delayed interfacial spallation during subsequent water immersion tests, performed up to one year after oxidation. Spallation was characterized by weight loss, the amount of spalled area, and acoustic emission response. Hydrogen annealing (prior to oxidation) reduced spallation both before and after immersion, but without measurably reducing the bulk sulfur content of the Y-doped alloys. The duration and frequency of sequential, co-located acoustic emission events implied an interfacial crack growth rate at least 10(exp -3) m/s, but possibly higher than 10(exp 2) m/s. This is much greater than classic moisture-assisted slow crack growth rates in bulk alumina (10(exp -6) to 10(exp -3) m/s), which may still have occurred undetected by acoustic emission. An alternative failure sequence is proposed: an incubation process for preferential moisture ingress leads to a local decrease in interfacial toughness, thus allowing fast fracture driven by stored strain energy.

Smialek, James L.↗

NASA NTRS1999

Carboxylic and dicarboxylic acids extracted from crushed magnesium oxide single crystals

Carboxylic and dicarboxylic acids (glycolic, oxalic, malonic and succinic) have been extracted with tetrahydrofuran (THF) and H2O from large synthetic MgO crystals, crushed to a medium fine powder. The extracts were characterized by infrared spectroscopy and 1H-NMR. The THF extracts were derivatized with tert-butyldimethylsilyl (t-BDMS) for GC-MS analysis. A single crystal separated from the extract was used for an x-ray structure analysis, giving the monoclinic unit cell, space group P21/c with ao = 5.543 A, bo = 8.845 A, co = 5.086 A, and beta = 91.9 degrees, consistent with beta-succinic acid, HOOC(CH2)COOH. The amount of extracted acids is estimated to be of the order of 0.1 to 0.5 mg g-1 MgO. The MgO crystals from which these organic acids were extracted grew from the 2860 degrees C hot melt, saturated with CO/CO2 and H2O, thereby incorporating small amounts of the gaseous components to form a solid solution (ss) with MgO. Upon cooling, the ss becomes supersaturated, causing solute carbon and other solute species to segregate not only to the surface but also internally, to dislocations and subgrain boundaries. The organic acids extracted from the MgO crystals after crushing appear to derive from these segregated solutes that formed C-C, C-H and C-O bonds along dislocations and other defects in the MgO structure, leading to entities that can generically be described as (HxCyOz)n-. The processes underlying the formation of these precursors are fundamental in nature and expected to be operational in any minerals, preferentially those with dense structures, that crystallized in H2O-CO2-laden environments. This opens the possibility that common magmatic and metamorphic rocks when weathering at the surface of a tectonically active planet like Earth may be an important source of abiogenically formed complex organic compounds.

NASA Discipline Exobiology↗

NASA NTRS2012

Deducing Wild 2 Components with a Statistical Dataset of Olivine in Chondrite Matrix

Introduction: A preliminary exam of the Wild 2 olivine yielded a major element distribution that is strikingly similar to those for aqueously altered carbonaceous chondrites (CI, CM, and CR) [1], in which FeO-rich olivine is preferentially altered. With evidence lacking for large-scale alteration in Wild 2, the mechanism for this apparent selectivity is poorly understood. We use a statistical approach to explain this distribution in terms of relative contributions from different chondrite forming regions. Samples and Analyses: We have made a particular effort to obtain the best possible analyses of both major and minor elements in Wild 2 olivine and the 5-30 micrometer population in chondrite matrix. Previous studies of chondrite matrix either include larger isolated grains (not found in the Wild 2 collection) or lack minor element abundances. To overcome this gap in the existing data, we have now compiled greater than 10(exp 3) EPMA analyses of matrix olivine in CI, CM, CR, CH, Kakangari, C2-ungrouped, and the least equilibrated CO, CV, LL, and EH chondrites. Also, we are acquiring TEM/EDXS analyses of the Wild 2 olivine with 500s count times, to reduce relative errors of minor elements with respect to those otherwise available. Results: Using our Wild 2 analyses and those from [2], the revised major element distribution is more similar to anhydrous IDPs than previous results, which were based on more limited statistics (see figure below). However, a large frequency peak at Fa(sub 0-1) still persists. All but one of these grains has no detectable Cr, which is dissimilar to the Fa(sub 0-1) found in the CI and CM matrices. In fact, Fa(sub 0-1) with strongly depleted Cr content is a composition that appears to be unique to Kakangari and enstatite (highly reduced) chondrites. We also note the paucity of Fa(sub greater than 58), which would typically indicate crystallization in a more oxidizing environment [3]. We conclude that, relative to the bulk of anhydrous IDPs, Wild 2 may have received a larger contribution from the Kakangari and/or enstatite chondrite forming regions. Alternatively, Wild 2 may have undergone accretion in an anomalously reducing region, marked by nebular condensation of this atypical forsterite. In [4], a similar conclusion was reached with an Fe-XANES study. We will also use similar lines of reasoning, and our previous conclusions in [5], to constrain the relative contributions of silicates that appear to have been radially transported from different ordinary and carbonaceous chondrite forming regions to the Kuiper Belt. In addition, the widespread depletion of Cr in these FeO-rich (Fa(sub greater than 20)) fragments is consistent with mild thermal metamorphism in Wild 2.

Frank, D. R.↗