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Promising route toward production of highly pure, finely divided, easily sinterable silicon nitride (Si3N4) involves thermal decomposition of silicon diimide {Si(NH)2} prepared by ammonolysis of Si(SCN)4 in CH3CN and purified by complete extraction of byproduct NH4SCN by use of ammonia at temperature and pressure above critical point.
Nitrogen is the second most abundant constituent of the Martian atmosphere, after CO2, present at a level of ca. 2.7 percent. Several authors have hypothesized that earlier in the planet's history, nitrogen was more abundant, but has been removed by processes such as exospheric loss from the atmosphere. However, an alternative sink for atmospheric nitrogen is the regolith; model calculations have predicted that, via the formation of NOx, HNO2 and HNO3 in the lower layers of the Martian atmosphere, the regolith might trap nitrite and nitrate anions, leading to the build-up of involatile nitrates. Integrated over 4.5 x 10(exp 9) yr, such a mechanism would contribute the equivalent of a layer of nitrates up to 0.3 cm thick distributed across the Martian surface. Features in thermal emission spectra of the surface of Mars have been interpreted tentatively as emanating from various anions (carbonates, bicarbonates, sulphates, etc.), and the presence of nitrates has also been addressed as a possibility. The identification of carbonates in SCN meteorites has allowed inferences to be drawn concerning the composition and evolution of the Martian atmosphere in terms of its carbon isotope systematics; if nitrites, nitrates, or other nitrogen-bearing salts could be isolated from SNC's, similar conclusions might be possible for an analogous nitrogen cycle. Nitrates are unstable, being readily soluble in water, and decomposed at temperatures between 50 C and 600 C, depending on composition. Any nitrates present in SNC's might be removed during ejection from the planet's surface, passage to Earth, or during the sample's terrestrial history, by weathering etc. The same might have been said for carbonates, but pockets of shock-produced glass (lithology C) from within the EET A79001 shergottite and bulk samples of other SNC contain this mineral, which did apparently survive. Nitrates occurring within the glassy melt pockets of lithology C in EET A79001 might likewise be protected. Lithology C glass was therefore selected for nitrate analysis, first by non-destructive infra red spectroscopy, and then by stepped combustion.
The circadian timing system (CTS) provides internal and external temporal coordination of an animal's physiology and behavior. In mammals, the generation and coordination of these circadian rhythms is controlled by a neural pacemaker, the suprachiasmatic nucleus (SCN), located within the hypothalamus. The pacemaker is synchronized to the 24 hour day by time cures (zeitgebers) such as the light/dark cycle. When an animal is exposed to an environment without time cues, the circadian rhythms maintain internal temporal coordination, but exhibit a 'free-running' condition in which the period length is determined by the internal pacemaker. Maintenance of internal and external temporal coordination are critical for normal physiological and psychological function in human and non-human primates. Exposure to altered gravitational environments has been shown to affect the amplitude, mean, and timing of circadian rhythms in species ranging from unicellular organisms to man. However, it has not been determined whether altered gravitational fields have a direct effect on the neural pacemaker, or affect peripheral parameters. In previous studies, the ability of a stimulus to phase shift circadian rhythms was used to determine whether a stimulus has a direct effect on the neural pacemaker. The present experiment was performed in order to determine whether acute exposure to a hyperdynamic field could phase shift circadian rhythms.
The synthesis and structure of the indium dithiocarbamate, In[SCN(CH3)2]3*1/2 4-mepy (4-mepy = 4-methylpyridine), is described. Indium metal was oxidized by tetramethylthiuramdisulfide in 4-methylpyridine at 25C to form a new, homoleptic indium(HI) dithiocarbamate in yields exceeding 60%. In[S2CN(CH3)213 exists as a discrete molecule with a distorted-octahedral geometry. The compound crystallizes in the P 1-bar (No. 2) space group with a = 9.282(l)A, b = 10.081(1)A, c = 12.502 A, alpha= 73.91 (1) degrees, beta = 70.21(1) degrees, gamma = 85.84(1) degrees, Z = 2,v(A(exp 3)) =1057.3(3), R = 0.046, and R(sub w) = 0.061.
The objective of the research is to quantitatively determine and understand the fundamental mechanisms that control the microstructural evolution during solidification of an assemblage of equiaxed dendritic crystals. A microgravity experiment will be conducted to obtain benchmark data on the transient growth and interaction of up to four equiaxed crystals of a pure and transparent metal analog (succinonitrile, SCN) under strictly diffusion dominated conditions. Of interest in the experiment are the transient evolution of the primary and secondary dendrite tip speeds, the dendrite morphology (i.e., tip radii, branch spacings, etc.) and solid fraction, the tip selection criterion, and the temperature field in the melt for a range of initial supercoolings and, thus, interaction "strengths" between the crystals. The experiment thus extends the microgravity measurements of Glicksman and coworkers for steady growth of a single dendrite [Isothermal Dendritic Growth Experiment (IDGE), first flown on USMP-2] to a case where growth transients are introduced due to thermal interactions between neighboring dendrites - a situation more close to actual casting conditions. Corresponding earth-based experiments will be conducted to ascertain the influence of melt convection. The experiments are supported by a variety of analytical models and numerical simulations. The data will primarily be used to develop and test theories of transient dendritic growth and the solidification of multiple interacting equiaxed crystals in a supercooled melt.
The Isothermal Dendritic Growth Experiment (IDGE) constituted a series of three NASA-supported microgravity experiments, all of which flew aboard the space shuttle, Columbia. This experimental space flight series was designed and operated to grow and record dendrite solidification in the absence of gravity-induced convective heat transfer, and thereby produce a wealth of benchmark-quality data for testing solidification scaling laws. The data and analysis performed on the dendritic growth speed and tip size in Succinontrie (SCN) demonstrates that although the theory yields predictions that are reasonably in agreement with experiment, there are significant discrepancies. However, some of these discrepancies can be explained by accurately describing the diffusion of heat. The key finding involves recognition that the actual three-dimensional shape of dendrites includes time-dependent side-branching and a tip region that is not a paraboloid of revolution. Thus, the role of heat transfer in dendritic growth is validated, with the caveat that a more realistic model of the dendrite then a paraboloid is needed to account for heat flow in an experimentally observed dendrite. We are currently conducting additional analysis to further confirm and demonstrate these conclusions. The data and analyses for the growth selection physics remain much less definitive. From the first flight, the data indicated that the selection parameter, sigma*, is not exactly a constant, but exhibits a slight dependence on the supercooling. Additional data from the second flight are being examined to investigate the selection of a unique dendrite speed, tip size and shape. The IDGE flight series is now complete. We are currently completing analyses and moving towards final data archiving. It is gratifying to see that the IDGE published results and archived data sets are being used actively by other scientists and engineers. In addition, we are also pleased to report that the techniques and IDGE hardware system that the authors developed with NASA, are being currently employed on both designated flight experiments, like EDSE, and on flight definition experiments, like TDSE.
Porosity in the form of "bubbles and pipes" can occur during controlled directional solidification processing of metal alloys. It is detrimental to material properties and precludes obtaining meaningful scientific results. On Earth, density differences allow an initiated bubble can rise through the liquid and "pop" at the surface resulting in a sound casting. This is not likely to occur in a microgravity environment and, unfortunately, a number of experiments conducted in microgravity have suffered from porosity effects. The current investigation is a systematic effort towards understanding porosity formation and mobility during controlled directional solidification in a microgravity environment. This will be investigated by utilizing a transparent material, succinonitrile (SCN), in conjunction with a translating temperature gradient stage so that direct observation and recording of pore generation and mobility can be made. The talk will cover the porosity problem, the details of the proposed experiments and the experimental hardware, and the expectations from the microgravity experiments.
The objective of the research is to quantitatively determine and understand the fundamental mechanisms that control the microstructural evolution during equiaxed dendritic solidification. A microgravity experiment will be conducted to obtain benchmark data on the transient growth and interaction of up to four equiaxed crystals of a pure and transparent metal analog (succinonitrile, SCN) under strictly diffusion-dominated conditions. Of interest in the experiment are the transient evolution of the primary and secondary dendrite tip speeds, the dendrite morphology and solid fraction, the tip selection criterion, and the temperature field in the melt for a range of interaction "strengths" between the crystals. The experiment extends the microgravity measurements of Glicksman and co-workers isothermal dendritic growth experiment (IDGE) for steady growth of a single dendrite to a case where growth transients are introduced due to thermal interactions between neighboring dendrites - a situation closer to actual casting conditions. Corresponding Earth-based experiments will be conducted to ascertain the influence of melt convection. The experiments are supported by a variety of analytical models and numerical simulations. The data will be used to develop and test theories of transient dendritic growth and the solidification of multiple interacting equiaxed crystals in a supercooled melt.
A space experiment, and supporting ground-based research, is proposed to study the microstructural evolution in free dendritic growth from a supercooled melt of the transparent model alloy succinonitrile-acetone (SCN-ACE). The research is relevant to equiaxed solidification of metal alloy castings. The microgravity experiment will establish a benchmark for testing of equiaxed dendritic growth theories, scaling laws, and models in the presence of purely diffusive, coupled heat and solute transport, without the complicating influences of melt convection. The specific objectives are to: determine the selection of the dendrite tip operating state, i.e. the growth velocity and tip radius, for free dendritic growth of succinonitrile-acetone alloys; determine the growth morphology and sidebranching behavior for freely grown alloy dendrites; determine the effects of the thermal/solutal interactions in the growth of an assemblage of equiaxed alloy crystals; determine the effects of melt convection on the free growth of alloy dendrites; measure the surface tension anisotropy strength of succinon itrile -acetone alloys establish a theoretical and modeling framework for the experiments. Microgravity experiments on equiaxed dendritic growth of alloy dendrites have not been performed in the past. The proposed experiment builds on the Isothermal Dendritic Growth Experiment (IDGE) of Glicksman and coworkers, which focused on the steady growth of a single crystal from pure supercooled melts (succinonitrile and pivalic acid). It also extends the Equiaxed Dendritic Solidification Experiment (EDSE) of the present investigators, which is concerned with the interactions and transients arising in the growth of an assemblage of equiaxed crystals (succinonitrile). However, these experiments with pure substances are not able to address the issues related to coupled heat and solute transport in growth of alloy dendrites.
Modeling solidification microstructures has become an area of intense study in recent years. The properties of large scale cast products, ranging from automobile engine blocks to aircraft components and other industrial applications, are strongly dependent on the physics that occur at the mesoscopic and microscopic length scales during solidification. The predominant morphology found in solidification microstructures is the dendrite, a tree-like pattern of solid around which solidification proceeds. The microscopic properties of cast products are determined by the length scales of these dendrites, and their associated segregation profiles. For this reason understanding the mechanisms for pattern selection in dendritic growth has attracted a great deal of interest from the experimental and theoretical communities. In particular, a great deal of research has been undertaken to understand such issues as dendrite morphology, shape and growth speed. Experiments on dendrite evolution in pure materials by Glicksman and coworkers on succinonitrile (SCN), and more recently pivalic acid (PVA), as well as other transparent analogs of metals, have provided tests of theories for dendritic growth, and have stimulated considerable theoretical progress. These experiments have clearly demonstrated that in certain parameter ranges the physics of the dendrite tip can be characterized by a steady value for the dendrite tip velocity, radius of curvature and shape. Away from the tip, the time-dependent dendrite exhibits a characteristic sidebranching as it propagates, which is not yet well understood. These experiments are performed by observing individual dendrites growing into an undercooled melt. The experiments are characterized by the dimensionless undercooling. Most experiments are performed at low undercooling.
The interaction of an insoluble particle with a growing solid-liquid interface (SLI) has been a subject of investigation for the four decades. For a metallurgist or a material scientist understanding the fundamental physics of such an interaction is relevant for applications that include distribution of reinforcement particles in metal matrix composites, inclusion management in castings, and distribution of Y2Ba1Cu1O5 (211) precipitates (flux pinning sites) in Y1Ba2Cu3O7 (123) superconducting crystals. The same physics is also applicable to other areas including geological applications (frost heaving in soils) and preservation of biological cells. Experimentally this interaction can be quantified in terms of a critical growth velocity, Vcr, of the SLI below which particles are pushed ahead of the advancing interface, and above which the particles are engulfed. Past experimental evidence suggests that this Vcr is an inverse function of the particle radius, R. In order to isolate the fundamental physics that governs such a relationship it is necessary to minimize natural convection at the SLI that is inherent in ground based experiments. Hence for the purpose of producing benchmark data (Vcr vs. R) PEP is a natural candidate for micro-gravity experimentation. Accordingly, experiments with pure Al containing a dispersion of ZrO2 particles and an organic analogue, succinonitrile (SCN) containing polystyrene particles have been performed on the LMS and USMP-4 mission respectively. In this paper we will summarize the experimental data that was obtained during these two micro-gravity missions and show that the results differ compared to terrestrial experiments. We will also discuss the basic elements of our analytical and numerical model and present a comparison of the predictions of these models against micro-gravity experimental data. Finally. we will discuss our future experimental plan that includes the ISS glovebox and MSRRl.
During the time period covered by this report, SAIC: 1) Continued to develop and assess processes and approaches that can be applied to Second Generation Reuseable Launch Vehicles (RLV) technologies prioritization. An approach based on the use of analytic Saaty scale functions has been defined and is being investigated. 2) Planned and facilitated technologies prioritization workshops, supported development of systems program algorithms based on the concept of influence diagramming, and assessment of analogies between aircraft and space systems developments. 3) Video interviews held with X-37 personnel at Dryden. The CD-ROM is being concluded and a near-final review disc is expected soon. 4) CD-ROMS were produced by Engineered Multimedia, Inc. (EMI) under subcontract to SAIC. These two CD-ROM products, "Microgravity" and "New Horizons", were delivered to MSFS technical representatives at a briefing at SAID on January 18, 2001. 5) Presentation brochure, "Aviation/Space Analog Team Interim Report" was provided to Space Propulsion Synergy Team (SPST) members and to NASA personnel. Wrap-up of effort will be a mid-April briefing to both MSFC and the full SPST membership. Support to Phase 2 of CCPD ends 3/31/01. Phase 3 continuation effort planned with emphasis on technical info content. 6) Recommended that eliminating the B-52 flights of the X-37 in favor of alternate approached be evaluated. Discovered that a required change to the thruster valves of the X-37 had not been made. Repair work continues on the lower fuselage section of the X-37, in the areas that experienced core collapse. The currently catalogued potential weight increases and decreases are about equal, but this does not include the impact of the cable weight underestimate reported earlier. The CFD for RCS testing correlates well with the wind tunnel data. 7) The Level IV CCB approved SCN-4 to the MC-1 Engine SPecification. Approved changes have been incorporated into the specification, and Revision D has been released to the Repository. Billy Gonterman, SAIC, traveled to SSC to perform a five-day readiness assessment on the progress of facilities activation. Implemented modifications to the MC-1 Engine TPA Component Database. 8) Replaced 25 Combined-Cycle Propulsion Database (CCPD) documents; modified the low-on screen to include a direct email link for user contact; prepared a summary presentation of current and proposed tasks.
Reactive sputtering was used to grow thin films of Sc(x)Ga(1-x)N with scandium concentrations of 20%-70% on quartz substrates at temperatures of 300-675 K. X-ray diffraction (XRD) of the films showed either weak or no structure, suggesting the films are amorphous or microcrystalline. Optical absorption spectra were taken of each sample and the optical band gap was determined. The band gap varied linearly with increasing Ga concentration between 2.0 and 3.5 eV. Ellipsometry was used to confirm the band gap measurements and provide optical constants in the range 250-1200 nm. ScN and GaN have different crystal structures (rocksalt and wurzite, respectively), and thus may form a heterogeneous mixture as opposed to an alloy. Since the XRD data were inconclusive, bilayers of ScN/GaN were grown and optical absorption spectra taken. A fundamental difference in the spectra between the bilayer films and alloy films was seen, suggesting the films are alloys, not heterogeneous mixtures.
Laser-ablated Sc and Ti atoms have been reacted with NO during condensation in excess argon. Matrix infrared spectra show that the major products are the side bonded Sc[NO] species and the inserted NScO and NTiO molecules based on isotopic substitution (15NI6O and 15N18O) and DIFT calculations of isotopic frequencies, which provide a match for two modes in three isotopic modifications for each molecule. The NScO and NTiO molecules are nitride/oxides with M-O stretching modes only 46-88/cm below the diatomic metal oxides but M-N stretching modes 314-442/cm lower than the diatomic metal nitride molecules. The ScN, ScO, TiN, and TiO molecules are observed as decomposition products. Evidence is also presented for the nitrosyls ScNO and TiNO, the Sc[NO]+ cation, and the NTiO- anion.
The displays for the Materials Conference presents some of the facilities and capabilities in SD46 that can be useful to a prospective researcher from University, Academia or other government labs. Several of these already have associated personnel as principal and co-investigators on NASA peer reviewed science investigations. 1. SCN purification facility 2. ESL facility 3. Static and Dynamic magnetic field facility 4. Microanalysis facility 5. MSG Investigation - PFMI 6. Thermo physical Properties Measurement Capabilities.
Porosity in the form of "bubbles and pipes" can occur during controlled directional solidification processing of metal alloys. It is detrimental to material properties and precludes obtaining meaningful scientific results. On Earth, density differences allow an initiated bubble can rise through the liquid and "pop" at the surface resulting in a sound casting. This is not likely to occur in a microgravity environment and, unfortunately, a number of experiments conducted in microgravity have suffered from porosity effects. The current investigation is a systematic effort towards understanding porosity formation and mobility during controlled directional solidification in a microgravity environment. This will be investigated by utilizing a transparent material, succinonitrile (SCN), in conjunction with a translating temperature gradient stage so that direct observation and recording of pore generation and mobility can be made. The talk will cover the porosity problem, the details of the proposed experiments and the experimental hardware, and the expectations from the microgravity experiments.
A new synthetic route to isothiocyanate-containing materials is presented. Eight isothiocyanate- 4-methylpyridine (y-picoline) compounds were prepared by refluxing metal powders (Mn, Fe, Co, Ni, and Cu) with thiourea in y-picoline. With the exception of compound 5,prepared with Co, the isothiocyanate ligand was generated in situ by the isomerization of thiourea to NH4+SCN- at reflux temperatures. The complexes were characterized by x-ray crystallography. Compounds 1,2, and 8 are the first isothiocyanate- 4-methylpyridine anionic compounds ever prepared and structurally characterized. Compounds 1 and 2 are isostructural with four equatorially bound isothiocyanate ligands and two axially bound y-picoline molecules. Compound 8 is a five-coordinate copper(II) molecule with a distorted square-pyramidal geometry. Coordinated picoline and two isothiocyanates form the basal plane and the remaining isothiocyanate is bound at the apex. Structural data are presented for all compounds.
The Materials Science Program is structured so that NASA s headquarters is responsible for the program content and selection, through the Enterprise Scientist, and MSFC provides for implementation of ground and flight programs with a Discipline Scientist and Discipline Manager. The Discipline Working Group of eminent scientists from outside of NASA acts in an advisory capacity and writes the Discipline Document from which the NRA content is derived. The program is reviewed approximately every three years by groups such as the Committee on Microgravity Research, the National Materials Advisory Board, and the OBPR Maximization and Prioritization (ReMaP) Task Force. The flight program has had as many as twenty-six principal investigators (PIs) in flight or flight definition stage, with the numbers of PIs in the future dependent on the results of the ReMaP Task Force and internal reviews. Each project has a NASA-appointed Project Scientist, considered a half-time job, who assists the PI in understanding and preparing for internal reviews such as the Science Concept Review and Requirements Definition Review. The Project Scientist also insures that the PI gets the maximum science support from MSFC, represents the PI to the MSFC community, and collaborates with the Project Manager to insure the project is well-supported and remains vital. Currently available flight equipment includes the Materials Science Research Rack (MSRR-1) and Microgravity Science Glovebox. Ground based projects fall into one or more of several categories. Intellectual Underpinning of Flight Program projects include theoretical studies backed by modeling and computer simulations; bring to maturity new research, often by young researchers, and may include preliminary short duration low gravity experiments in the KC-135 aircraft or drop tube; enable characterization of data sets from previous flights; and provide thermophysical property determinations to aid PIs. Radiation Shielding and preliminary In Situ Resource Utilization (ISRU) studies work towards future long duration missions. Biomaterials support materials issues affecting crew health. Nanostructured Materials are currently considered to be maturing new research, and Advanced Materials for Space Transportation has as yet no PIs. PIs are assigned a NASA Technical Monitor to maintain contact, a position considered to be a 5 percent per PI effort. Currently 33 PIs are supported on the 1996 NRA, which is about to expire, and 59 on the 1998 NRA. Two new NRAs, one for Radiation Shielding and one for Materials Science for Advanced Space Propulsion are due to be announced by the 2003 fiscal year. MSFC has a number of facilities supporting materials science. These include the Microgravity Development Laboratory/SD43; Electrostatic Levitator Facility; SCN Purification Facility; Electron Microscope/Microprobe Facility; Static and Rotating Magnetic Field Facility; X-Ray Diffraction Facility; and the Furnace Development Laboratory.