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NASA NTRS1992

Effect of strain and stress on the relative dimensions of the 'hard' and 'soft' regions in crept NaCl single crystals

It is shown that the L exp h and L exp s ratio, where these are respectively the average dimensions of the hard and soft regions as a function of stress and strain in crept NaCl single crystals, significantly influences the steady-state creep and power-law breakdown in these crystals. This is suggested to be due to a change in the internal stresses of the material. The present observations also indicate that steady-state creep is more likely to be influenced by the degree of refinement in the cell boundaries within the subgrains than by the formation of equiaxed subgrains under power-law conditions.

S. V. Raj↗

NASA NTRS1989

On the stability of the creep substructure in NaCl single crystals

Microstructural observations were conducted on NaCl single crystals after creep. The microstructure after a stress increase followed by a stress decrease consisted primarily of cells; no significant number of subgrains were observed although they were present in the microstructures produced during uninterrupted tests. Prestraining in the exponential creep regime produced an uniform distribution of dislocations and a few subboundaries which transformed to equiaxed subgrains when tested in the power law creep region. This substructure was similar to that observed in an as-received specimen deformed to an equivalent strain. Prior creep in the power law creep region produced equiaxed subgrains whose boundaries were found to be mechanically stable when the specimen was retested in the exponential creep region. The role of subboundary migration in the formation of new subgrains is discussed.

Raj, S. V.↗

NASA NTRS1991

High resolution X-ray diffraction imaging of lead tin telluride

High resolution X-ray diffraction images of two directly comparable crystals of lead tin telluride, one Bridgman-grown on Space Shuttle STS 61A and the other terrestrially Bridgman-grown under similar conditions from identical material, present different subgrain structure. In the terrestrial, sample 1 the appearance of an elaborate array of subgrains is closely associated with the intrusion of regions that are out of diffraction in all of the various images. The formation of this elaborate subgrain structure is inhibited by growth in microgravity.

Steiner, Bruce↗

NASA NTRS1992

Environmental fatigue of an Al-Li-Cu alloy. Part 3: Modeling of crack tip hydrogen damage

Environmental fatigue crack propagation rates and microscopic damage modes in Al-Li-Cu alloy 2090 (Parts 1 and 2) are described by a crack tip process zone model based on hydrogen embrittlement. Da/dN sub ENV equates to discontinuous crack advance over a distance, delta a, determined by dislocation transport of dissolved hydrogen at plastic strains above a critical value; and to the number of load cycles, delta N, required to hydrogenate process zone trap sites that fracture according to a local hydrogen concentration-tensile stress criterion. Transgranular (100) cracking occurs for process zones smaller than the subgrain size, and due to lattice decohesion or hydride formation. Intersubgranular cracking dominates when the process zone encompasses one or more subgrains so that dislocation transport provides hydrogen to strong boundary trapping sites. Multi-sloped log da/dN-log delta K behavior is produced by process zone plastic strain-hydrogen-microstructure interactions, and is determined by the DK dependent rates and proportions of each parallel cracking mode. Absolute values of the exponents and the preexponential coefficients are not predictable; however, fractographic measurements theta sub i coupled with fatigue crack propagation data for alloy 2090 established that the process zone model correctly describes fatigue crack propagation kinetics. Crack surface films hinder hydrogen uptake and reduce da/dN and alter the proportions of each fatigue crack propagation mode.

Piascik, Robert S.↗

NASA NTRS1991

The effect of zinc additions on the environmental stability of Alloy 8090 (Al-Li-Cu-Mg-Zr)

Stress corrosion cracking (SCC) remains a problem in both Al-Li and conventional Al heat treatable alloys. It has recently been found that relatively small additions (less than or approximately 1 wt-percent) of Zn can dramatically improve the SCC performance of alloy 8090 (Al-Li-Cu-Mg-Zr). Constant load time to failure experiments using cylindrical tensile samples loaded between 30 and 85 percent of TYS indicate improvements of orders of magnitude over the baseline 8090 for the Zn-containing alloys under certain aging conditions. However, the toughnesses of the alloys were noticeably degraded due to the formation of second phase particles which primarily reside on grain and subgrain boundaries. EDS revealed that these intermetallic particles were Cu and Zn rich. The particles were present in the T3 condition and were not found to be the result of quench rate, though their size and distribution were. At 5 hours at 160 C, the alloys displayed the greatest susceptibility to SCC but by 20 hours at 160 C the alloys demonstrated markedly improved TTF lifetimes. Aging past this time did not provide separable TTF results, however, the alloy toughnesses continued to worsen. Initial examination of the alloys microstructures at 5 and 20 hours indicated some changes most notably the S' and delta' distributions. A possible model by which this may occur will be explored. Polarization experiments indicated a change in the trend of E(sub BR) and passive current density at peak aging as compared to the baseline 8090. Initial pitting experiments indicated that the primary pitting mechanism in chloride environments is one occurring at constituent (Al-Fe-Cu) particles and that the Cu and Zn rich boundary precipitates posses a breakaway potential similar to that of the matrix acting neither anodic or cathodic in the first set of aerated 3.5 w/o NaCl experiments. Future work will focus on the identification of the second phase particles, evaluation of K(sub 1SCC) and plateau da/dt via both DCB and slow strain rate techniques. A lower Zn content variant will be examined in the near future in hopes of optimizing toughness, density and SCC performance.

Kilmer, Raymond J.↗

NASA NTRS2019

In Situ Observation of Growth Dynamics in DECLIC Directional Solidification Insert Onboard ISS: DSI-R Flight Campaign

The study of solidification microstructure formation is of utmost importance for materials design and processing, as solid-liquid interface patterns largely govern mechanical and physical properties. Pattern selection occurs under dynamic conditions of growth in which the initial morphological instability evolves nonlinearly and undergoes a reorganization process. The dynamic and nonlinear nature of this instability renders in situ observation of the interface an invaluable tool to gain knowledge on the time-evolution of the interface pattern. Transparent organic analogs, which solidify like metallic alloys, allow direct visualization of interface dynamics. Extensive ground-based studies of both metallic and organic bulk samples have established the presence of significant convection during solidification processes that alters the formation of interfacial microstructures. A reduced-gravity environment is therefore mandatory for fluid flow elimination in bulk samples. In the framework of the CNES project MISOL3D (MIcrostrutures de SOLidification 3D) and the NASA projects DSIP (Dynamical Selection of 3D Interface Patterns), SPADES (SPAtiotemporal Evolution of three-dimensional DEndritic array Structures) and CAMUS (ComputAtional Studies of MicrostrUcture Formation During Alloy Solidification in Microgravity), we participated in the development of the Directional Solidification Insert (DSI) of the DEvice for the study of Critical Liquids and Crystallization (DECLIC). The DECLIC-DSI is dedicated to in situ and real-time characterization of solid-liquid interface patterns during directional solidification of transparent alloys in diffusive transport regime. Between April 2010 and March 2011, the first ISS campaign (DSI) explored the entire range of microstructures resulting in unprecedented observations. A second campaign (DSI-R), performed between October 2017 and December 2018, in which the insert contained an alloy of higher solute concentration, allowed to complete the benchmark database. The increase of solute concentration resulted in well-developed dendritic patterns at lower velocities (lower interface curvature and larger tip radius). The microstructure resulting from dendritic growth is dominant in metallurgy so that it is fundamental to understand the mechanisms of its formation. The main aims of this experimental campaign are to understand: the mechanisms of the cell to dendrite transition, the fundamental mechanisms of sidebranching formation, the dependence of dendrite tip shapes on growth conditions, the interaction of primary array and secondary sidebranches, and the influence of subgrain boundaries on the spatiotemporal organization of the array structure. Preparation, analysis and interpretation of the experiments performed onboard ISS are considerably enhanced by experiments performed on ground using thin-samples (Pr. Trivedi’s group) and phase-field simulations of microstructure formation in a diffuse growth regime (Pr. Karma’s group). In this summary, we will present an initial assessment of the results obtained during the DSI-R campaign. Nomenclature Vp: pulling velocity G: thermal gradient L: solidified length rtip: tip curvature radius Acronyms/Abbreviations CADMOS: Centre d'Aide au Développement des activités en Micro-pesanteur et des Opérations Spatiales CNES: Centre National d’Études Spatiales DECLIC: Device for the study of Critical LIquids and Crystallization DSI: Directional Solidification Insert DSI-R: Directional Solidification Insert - Refurbish ISS: International Space Station NASA: National Aeronautics and Space Administration PF: phase-field SCN: Succinonitrile 3D: three-dimensional

Mota, F.L.↗

NASA NTRS1992

Effect of temperature on the formation of creep substructure in sodium chloride single crystals

The effect of temperature on the substructure morphology and the cell and subgrain size was investigated experimentally in NaCl single crystals under creep in the temperature range 573-873 K. It is found that the effect of temperature on the cell and subgrain sizes is weak in comparison with the effect of stress. However, there was a qualitative change in the substructure morphology with temperature, with the cells and subgrains better defined at higher temperatures. The volume fraction of the cell boundaries decreased with increasing temperature, thereby indicating a refinement of the microstructure at higher temperatures.

Raj, Sai V.↗

NASA NTRS1981

The physics of creep and attenuation in the mantle

The objective is to investigate the role of dislocations in both creep and attenuation. Attenuation in the mantle at seismic frequencies is thought to be caused by the glide of dislocations in the subgrains. Both kink and impurity drag can contribute to the glide time constant. The kink-formation, or Peierls barrier, model for dislocation glide is seen as a low-temperature, high-frequency mechanism most appropriate for pure systems. It is noted that a small amount of impurity drag brings the dislocation glide characteristic time into the seismic band at upper-mantle temperatures. The attenuation and creep behavior of the mantle are related by way of the dislocation structure. Analysis of the various possible mechanisms is facilitated by casting them and the geophysical data in terms of a pre-exponential characteristic time and an activation energy.

Anderson, D. L.↗

NASA NTRSDate not supplied

Three-dimensional in Situ Observations of Polycrystalline Microstructure Evolution During Directional Solidification of Transparent Alloys Aboard the ISS and Quantitative Comparison with Numerical Modeling

Cellular/dendritic microstructures formed during solidification have a crucial influence on the mechanical properties of a wide range of structural alloys. By minimizing the amount of gravity-induced convection in the liquid, directional solidification experiments using transparent organic alloys conducted in the DECLIC-DSI onboard the International Space Station have provided unique 3D in situ observations of the spatiotemporal evolution of the solid-liquid interface during the formation of cellular and dendritic microstructures under purely diffusive growth conditions in polycrystalline samples containing several grains with a small misorientation with respect to the temperature gradient. Those observations have made it possible to perform benchmark quantitative comparisons with the predictions of state-of-the-art phase-field simulations of microstructure formation in 3D on experimentally relevant length and time scales. This talk will report quantitative comparisons between microgravity experiments and phase-field simulations in succinonitrile-camphor alloys of two different compositions that shed new light on the role of subgrain boundaries in the spatiotemporal evolution of the primary cellular spacing and the selection of dendritic array structures.

Kaihua Ji↗

NASA NTRS2005

Surface and Internal Structure of Pristine Presolar Silicon Carbide

Silicon carbide is the most well-studied type of presolar grain. Isotope measurements of thousands [1,2] and structural data from over 500 individual grains have been reported [3]. The isotope data indicate that approximately 98% originated in asymptotic giant branch stars and 2% in supernovae. Although tens of different polytypes of SiC are known to form synthetically, only two polytypes have been reported for presolar grains. Daulton et al. [3] found that for SiC grains isolated from Murchison by acid treatments, 79.4% are 3C cubic beta-SiC, 2.7% are 2H hexagonal alpha-SiC, 17.1% are intergrowths of and , and 0.9% are heavily disordered. They report that the occurrence of only the and polytypes is consistent with the observed range of condensation temperatures of circumstellar dust for carbon stars. Further constraint on the formation and subsequent alteration of the grains can be obtained from studies of the surfaces and interior structure of grains in pristine form, i.e., prepared without acid treatments [4,5]. The acid treatments remove surface coatings, produce etch pits around defect sites and could remove some subgrains. Surface oxides have been predicted by theoretical modeling as a survival mechanism for SiC grains exposed to the hot oxidizing solar nebula [6]. Scanning electron microscopy studies of pristine SiC shows some evidence for the existence of oxide and organic coatings [4]. We report herein on transmission electron microscopy studies of the surface and internal structure of two pristine SiC grains, including definitive evidence of an oxide rim on one grain, and the presence of internal TiC and AlN grains.

Stroud, Rhonda, M.↗

NASA NTRSDate not supplied

Three-Dimensional In Situ Observations of Polycrystalline Microstructure Evolution During Directional Solidification of Transparent Alloys Aboard the ISS and Quantitative Comparison with Numerical Modeling

Cellular/dendritic microstructures formed during solidification have a crucial influence on the mechanical properties of a wide range of structural alloys. By minimizing the amount of gravity-induced convection in the liquid, directional solidification experiments using transparent organic alloys conducted in the DECLIC-DSI onboard the International Space Station have provided unique 3D in situ observations of the spatiotemporal evolution of the solid-liquid interface during the formation of cellular and dendritic microstructures under purely diffusive growth conditions. Those observations have made it possible to perform benchmark quantitative comparisons with the predictions of state-of-the-art phase-field simulations of microstructure formation in 3D on experimentally relevant length and time scales. This talk will report quantitative comparisons between microgravity experiments and phase-field simulations in succinonitrile-camphor alloys of two different compositions, which shed new light on the selection of dendritic array structures, and on roles of macroscopic curvatures and subgrain boundaries between grains with a small misorientation with respect to the temperature gradient in the spatiotemporal evolution of the primary cellular spacing.

Kaihua Ji↗

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 NTRS1998

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 (THE) and H2O from large synthetic MgO crystals, crushed to a medium fine powder. The extracts were characterized by infrared spectroscopy and (sup 1)H-NMR (Nuclear Magnetic Resonance). The THF extracts were derivatized with tert-butyldimethylsilyl (t-BDMS) for GC-MS (Gas Chromatography - Mass Spectroscopy) analysis. A single crystal separated from the extract was used for an x-ray structure analysis, giving the monoclinic unit cell, space group P2(sub 1)/c with a(sub o) = 5.543 A, b(sub o) = 8.845 A, c(sub o) = 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 MgO. The MgO crystals from which these organic acids were extracted grew from the 2360 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)(sup 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.

Freund, Friedemann↗

NASA NTRS1988

Structural anomalies in undoped Gallium Arsenide observed in high resolution diffraction imaging with monochromatic synchrotron radiation

Novel, streak-like disruption features restricted to the plane of diffraction have recently been observed in images obtained by synchrotron radiation diffraction from undoped, semi-insulating gallium arsenide crystals. These features were identified as ensembles of very thin platelets or interfaces lying in (110) planes, and a structural model consisting of antiphase domain boundaries was proposed. We report here the other principal features observed in high resolution monochromatic synchrotron radiation diffraction images: (quasi) cellular structure; linear, very low-angle subgrain boundaries in (110) directions, and surface stripes in a (110) direction. In addition, we report systematic differences in the acceptance angle for images involving various diffraction vectors. When these observations are considered together, a unifying picture emerges. The presence of ensembles of thin (110) antiphase platelet regions or boundaries is generally consistent not only with the streak-like diffraction features but with the other features reported here as well. For the formation of such regions we propose two mechanisms, operating in parallel, that appear to be consistent with the various defect features observed by a variety of techniques.

Steiner, B.↗

NASA NTRS1989

Structural anomalies in undoped gallium arsenide observed in high-resolution diffraction imaging with monochromatic synchrotron radiation

Steiner, B.↗

NASA NTRS1989

Creep substructure formation in sodium chloride single crystals in the power law and exponential creep regimes

Creep tests conducted on NaCl single crystals in the temperature range from 373 to 1023 K show that true steady state creep is obtained only above 873 K when the ratio of the applied stress to the shear modulus is less than or equal to 0.0001. Under other stress and temperature conditions, corresponding to both power law and exponential creep, the creep rate decreases monotonically with increasing strain. The transition from power law to exponential creep is shown to be associated with increases in the dislocation density, the cell boundary width, and the aspect ratio of the subgrains along the primary slip planes. The relation between dislocation structure and creep behavior is also assessed.

Raj, S. V.↗

NASA NTRS2013

Organic Nano-Grains in Comet 103P/Hartley 2: The Organic Glue of Porous Aggregate Grains?

The GNIRS instrument on the Gemini 8-‐m telescope observed comet 103P/Hartley on 2010-‐ Dec-‐04UT, a month after the EPOXI Mission encounter, and detected the 3.3 and 3.4 um bands in emission. The 3.3/3.4 ratio and the broad band widths are consistent with experiments of heated (approximately 600 K) aliphatic carbon (-CH3, -CH2) thin films. For the 3.4 micron band to be in emission, the aliphatic bonds must be attached to a carrier possessing the strongly UV-‐absorbing C=C aromatic rings, and these rings have to be less than 50-‐100 carbon atoms (4-6 Angstrom) for attached -CH bonds to also generate a 3.3 micron-band in emission. Slightly larger (≥10Å) Very Small Grains (VSGs) can absorb single UV photons comparable to or exceeding their heat capacity, thermally fluctuate and release IR photon(s). The 3.3 micron and 3.4 micron bands observed by GNIRS suggest that organic macromolecules/ nano-‐grains with both aliphatic and aromatic bonds are fluorescing/thermally fluctuating in the coma. Aliphatic and aromatic materials have been seen in Stardust samples and the primitive carbonaceous chondrite 'Tagish Lake'. The larger the ratio of the -CH2/-CH3 components of the aliphatic 3.4 micron band, the more 'primitive' the organic material. In a Stardust organic globule, some aliphatic bonds were transformed into aromatic bonds during the low dosage of Transmission Electron Microscope imaging. Conversely, lab experiments show irradiation of ices containing small PAHs generates aliphatic organics. Photo-‐processing of ices also likely forms the ubiquitous aliphatic coatings that appear on the surfaces of all silicate subgrains constituting nine cometary interplanetary dust particles. The aliphatic coatings, dominated by -CH2, likely were important in sticking the aggregates together, and existed prior to incorporation of dust aggregates into comet nuclei. These comet aliphatics may be some of the sought-‐after precursors to the more robust and complex organics studied as Insoluble Organic Matter in carbonaceous chondrites. Aliphatic coatings on submicron grains, however, will not be observable in absorption because they are fairly transparent, nor do the aliphatic carbonaceous coatings produce the 3.4 micron emission band because the particles they are attached to are too large (too many vibration modes). We must probe the nano-‐sized organic carriers that undergo substantive thermal fluctuations in cometary comae and emit at 3.3 3.4 micron. Observations of the 3.3 and 3.4 micron emission features contribute to characterizing the evolution of organics prior to their incorporation into cometary nuclei as well as their rapid evolution in cometary comae, which in turn contributes to deepening our understanding of the evolution of organics on the surfaces of asteroids and outer icy bodies in our solar system. Studying organics in comets contributes to understanding the formation and evolution pathways of ISM organics through to the formation of the robust insoluble organic matter in meteorites. A'Hearn, M.F., et al. 2011, Science, 332, 1396; Bockelee-‐Morvan, D. et al. 1995, Icarus, 116, 18; De Gregorio, B.T., et al. 2010, GCA, 74, 4454; Dello Russo, N., et al. 2011, ApJ, 734, L8; Dischler et al. 1983, Solid State Communications, 48, 105; Flynn, G., et al. 2010a, LPSC, 41, #1079; Flynn, G., et al. 2010b, COSPAR, 38, F31-‐0012-‐10; Flynn, G., Wirick, S. 2011, LPSC, 42, #1856; Fomenkova, et al. 1994, GCA 58, 4503; Matrajt, G., et al. 2013, ApJ, 765, 145; Schutte, et al. 1993, ApJ, 415, 397; Wooden, D.H. et al. 2011, EPSC-‐DPS, 1557; Wooden, D.H. et al. 2013, submitted.

Stardust samples↗

NASA NTRS1997

Observational Evidence for Mixing and Dust Condensation in Core-Collapse Supernovae

Recent findings of isotopic anomalies of Ca-44 (the decay product of Ti-44) and the enhanced ratio of Si-28/Si-30 in SiC grains X, TiC subgrains, and graphite dust grains within primitive meteorites provides strong evidence that these presolar grains came from core-collapse supernovae. The chemical composition of the presolar grains requires macroscopic mixing of newly nucleo-synthesized elements from explosive silicon burning at the innermost zone of the ejects to higher velocities where C exists and where C/O > 1 in either the outer edge of the oxygen zone or in the He-C zone. To date, the only core-collapse supernova observed to form dust is the brightest supernova of the past four centuries, SN1987A in the Large Magellanic Cloud. Observations of SN1987A confirm large scale macroscopic mixing occurs in the explosions of massive stars. Rayleigh-Taylor instabilities macroscopically mix most of the ejects into regions which are still chemically homogeneous and which cool with different time scales. Only small clumps in the ejects are microscopically mixed. Observations show that dust condensed in the ejects of SN1987A after approx.500 days in the Fe-rich gas. Neither silicates nor SiC grains were seen in the dust emission spectrum of SN1987A. SN1987A, the Rosetta Stone of core-collapse supernovae, shows that while the mixing required to explain presolar grains occurs, the rapid cooling of the Fe zone and the sustained high temperatures of the O-Si, O-C, and He-C zones favor the formation of iron-rich rather than oxygen- or carbon-rich grains.

Wooden, Diane↗