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At least 73 records · Page 4

Material Science Experiments on Mir

This paper describes the microgravity materials experiments carried out on the Shuttle/Mir program. There were six experiments, all of which investigated some aspect of diffusivity in liquid melts. The Liquid Metal Diffusion (LMD) experiment investigated the diffusivity of molten Indium samples at 185 C using a radioactive tracer, In-114m. By monitoring two different gamma ray energies (190 keV and 24 keV) emitted by the samples it was possible to measure independently the diffusion rates in the bulk and at the surface of the samples. The Queens University Experiment in Liquid Diffusion (QUELD) was the furnace facility used to process 213 samples for the five other experiments. These experiments investigated the diffusion, ripening, crystal growth, and glass formation in metal, semiconductor, and glass samples. This facility had the capability to process samples in an isothermal or gradient configuration for varying periods of time at temperatures up to 900 C. Both the LMD and the QUELD furnaces were mounted on the Microgravity Isolation Mount (MIM) which provided isolation from g-jitter. All the microgravity experiments were supported by the Space Acceleration Measurement System (SAMS); a three head three axes acceleration monitoring system which measured and recorded the acceleration environment.

Kroes, Roger L.↗

Laboratory Investigation of the Effect of Venusian Weathering on Mineral Spectra

Introduction: The recent selection of two missions to Venus has renewed the importance of deter-mining weathering reactions between minerals and the Venusian atmosphere, and the spectral signatures of minerals before, during, and after these reactions. The rate at which weathering reactions progress also constrain show long unstable minerals will be present on the surface (e.g., [1]), and enables the use of mineralogy as a constraint on surface age(e.g., [2-3]).In order to gain an understanding of how mineral compositions and spectra change with weathering, we have begun conducting experiments in a 1 atm experimental setup at Wesleyan University. This setup exposes minerals to the temperature and most abundant gases of the Venus atmosphere (CO2, SO2, N2).We conducted initial experiments using biotite, calcite, and montmorillonite in order to test our methodology with minerals that may be relevant to recording the history of water on Venus. Methods: Experiments were conducted in Thermo Fisher Scientific Lindberg/Blue M Mini-Mite horizontal tube furnaces at Wesleyan University. Experiments used natural mineral chips and powders, and were conducted at 1 atmosphere and 460 °C under pre-mixed gases provided by Air Gas(Table 1). The furnaces are set up in a flow through configuration so that solid samples are exposed to a fixed gas composition, and quartz glass process tubes were used in all experiments (1/4” diameter for experiment V4, ½” diameter for all others). These conditions were maintained for the du-rations listed in Table 1, at which point the furnace was turned off with gas flowing until the sample was cool enough to extract under N2and be placed in a desiccator for storage. Run products were carbon coated and examined using a Hitachi SU5000 Field Emission Gun Scanning Electron Microscope (SEM) equipped with an EDAX Octane Pro EDS detector located at Wesley-an University. Visible-Near Infrared Spectroscopy (VNIR) analysis was performed on powdered samples under a nitrogen atmosphere using an ASD Fieldspec Proover the 350-2500 nm range. Powdered mineral samples were milled to a particle size of < 45μm and were spiked with an internal standard (Al2O3, corundum) to obtain quantitative mineralogy. Samples were analyzed using a Panalytical X’Pert pro X-ray Diffractometer (XRD), with an X’Celerator high speed detector and Co Kα radiation, with data collected at a step size of 0.02 ̊/minute step counting rate from 2 to 80 degrees 2θ at 45 mA/40kV in the X-ray Diffraction Laboratory located at NASA Johnson Space Center. Materials Data Inc (MDI) software suite, JadeTMv9 was used for Rietveld refinement to determine phase abundances and mineral identification by comparing XRD patterns to International Center for Diffraction Data (ICDD) database patterns. Table 1: Experimental matrix. Experiment Name Duration (Days)Gas Com-position (trace gas)MineralsV487SO2/N2(1.4%)Montmorillonite, biotiteV519SO2/N2(1.4%)CalciteV619CO2/SO2/N2(1.4% SO2, 2.1% N2)Montmorillonite, biotiteV828SO2/N2(1.4%)Biotite, calcite Results: Calcite. In both experiments, calcite was exposed to the SO2/N2gas mixture, and in both experimental run products, XRD analysis detected anhydrite, which is consistent with EDS measurements conducted in the SEM. The XRD analyses show greater amounts of anhydrite present after 28 days than 19, suggesting the calcite reaction progressed further given longer duration. Grain surface morphology as seen in the SEM also shows secondary mineral growth (Fig. 1). VNIR spectra show no change, as expected since anhydrite lacks spectral features in this wavelength range. Montmorillonite. Montmorillonite was exposed to two different gas mixtures, the SO2/N2mix and CO2/SO2/N2mix over different durations (87 and 19 days, respectively). VNIR analyses of both run products show a reduction in the 1441and1910 nm water features as well as a shift of the 1411 and 2011 nm features to shorter wavelengths that may indicate re-structuring in the crystal lattice and the production of amorphous phases [4]. XRD results are consistent with this, showing a shift of the 001 peak from 15Åto 10Åin both run products. The amount of X-ray amorphous material in the montmorillonite run products was greater than that present in the unreacted clay, being the greatest in the 87 day V4 experiment. No other secondary phases were detected in the run products, however sulfur was present in EDS analyses of powder samples.

A R Santos↗

Emittance Measurements at the Langley Chemical Physics Laboratory

Total hemispherical emittance measurements are made routinely for materials which may be heated by electrical resistance methods over the temperature range of 600 degrees to 2,000 F by using a black-body reference method. This employs a conical black body and a thermopile detector with a calcium fluoride lens. Emittance is obtained by measuring the radiant flux from the specimen strip and comparing it with the flux from an equal area of the black-body cone at the same temperature. The temperature measurements are made by use of thermocouples. It is planned to extend the temperature range of this type of measurement to temperatures above 2,000 F. Another technique has been investigated for measuring emittance of materials not amenable to electrical heating or thermocouple attachment. This method uses a black-body-cavity furnace similar to that used in reference 5 to measure emittance of transparent materials such as glass. The method employs a heated black-body cavity in which the semicircular specimen is allowed to come to the equilibrium temperature of the cavity and then is rotated in front of a water-cooled viewing port where a sensitive thermistor detector alternately views the specimen surface and the black-body cavity. The ratio of the two readings gives the specimen emittance directly, for the temperature of the black body. The detector output is recorded on a fast Brown self-balancing potentiometer. The furnace is provided with a water-cooled blackened shutter which may be inserted behind the specimen to eliminate any transmitted black-body radiation if the specimen is transparent. This apparatus is capable of measuring total normal emittance over the temperature range of 1,000 degrees to 2,000 F. Preliminary data for boron nitride specimens of two thicknesses are shown where total normal emittance is plotted against temperature for two experimental conditions: (1) black-body radiation incident on the back of the specimen and (2) no black-body radiation incident on the back of the specimen (that is, with a watercooled shutter behind the specimen). The data appear to indicate a slight transparency for the thin specimen and emittances of from 0.7 to 0.8 over the temperature range.

Lewis, B. W.↗

Kinetics of Nucleation and Crystal Growth in Glass Forming Melts in Microgravity

This flight definition project has the specific objective of investigating the kinetics of nucleation and crystal growth in high temperature inorganic oxide, glass forming melts in microgravity. It is related to one of our previous NASA projects that was concerned with glass formation for high temperature containerless melts in microgravity. The previous work culminated in two experiments which were conducted aboard the space shuttle in 1983 and 1985 and which consisted of melting (at 1500 C) and cooling levitated 6 to 8 mm diameter spherical samples in a Single Axis Acoustic Levitator (SAAL) furnace. Compared to other types of materials, there have been relatively few experiments, 6 to 8, conducted on inorganic glasses in space. These experiments have been concerned with mass transport (alkali diffusion), containerless melting, critical cooling rate for glass formation, chemical homogeneity, fiber pulling, and crystallization of glass forming melts. One of the most important and consistent findings in all of these experiments has been that the glasses prepared in microgravity are more resistant to crystallization (better glass former) and more chemically homogeneous than equivalent glasses made on Earth (1 g). The chemical composition of the melt appears relatively unimportant since the same general results have been reported for oxide, fluoride and chalcogenide melts. These results for space-processed glasses have important implications, since glasses with a higher resistance to crystallization or higher chemical homogeneity than those attainable on Earth can significantly advance applications in areas such as fiber optics communications, high power laser glasses, and other photonic devices where glasses are the key functional materials.

Day, Delbert E.↗

Kinetics of Nucleation and Crystal Growth in Glass Forming Melts in Microgravity

This flight definition project has the specific objective of investigating the kinetics of nucleation and crystal growth in high temperature inorganic oxide, glass forming melts in microgravity. It is related to one1 of our previous NASA projects that was concerned with glass formation for high temperature containerless melts in microgravity. The previous work culminated in two experiments which were conducted aboard the space shuttle in 1983 and 1985 and which consisted of melting (at 1500 C) and cooling levitated 6 to 8 mm diameter spherical samples in a Single Axis Acoustic Levitator (SAAL) furnace. Compared to other types of materials, there have been relatively few experiments, 6 to 8, conducted on inorganic glasses in space. These experiments have been concerned with mass transport (alkali diffusion), containerless melting, critical cooling rate for glass formation, chemical homogeneity, fiber pulling, and crystallization of glass forming melts. One of the most important and consistent findings in all of these experiments has been that the glasses prepared in microgravity are more resistant to crystallization (better glass former) and more chemically homogeneous than equivalent glasses made on earth (1g). The chemical composition of the melt appears relatively unimportant since the same general results have been reported for oxide, fluoride and chalcogenide melts. These results for space-processed glasses have important implications, since glasses with a higher resistance to crystallization or higher chemical homogeneity than those attainable on earth can significantly advance applications in areas such as fiber optics communications, high power laser glasses, and other photonic devices where glasses are the key functional materials. The classical theories for nucleation and crystal growth for a glass or melt do not contain any parameter that is directly dependent upon the g-value, so it is not readily apparent why glasses prepared in microgravity should be more resistant to crystallization than equivalent glasses prepared on earth. Similarly, the gravity-driven convection in a fluid melt is believed to be the primary force field that is responsible for melt homogenization on earth. Thus, it is not obvious why a glass prepared in space, where gravity-driven convection is ideally absent, would be more chemically homogeneous than a glass identically prepared on earth. The primary objective of the present research is to obtain experimental data for the nucleation rate and crystal growth rate for a well characterized silicate melt (lithium disilicate) processed entirely in space (low gravity) and compare these rates with the nucleation and crystal growth rates for a similar glass prepared identically on earth (1g).

Day, Delbert E.↗

Glass shell manufacturing in space

Highly-uniform, hollow glass spheres, which are used for inertial-confinement fusion targets, are formed from metal-organic gel powder feedstock in a drop-tower furnace. The modelling of this gel-to-sphere transformation has consisted of three phases: gel thermochemistry, furnance-to-gel heat transfer, and gravity-driven degradation of the concentricity of the molten shell. The heat transfer from the furnace to the free-falling gel particle was modelled with forced convection. The gel mass, dimensions, and specific heat as well as furnace temperature profile and furnace gas conductivity, were controlled variables. This model has been experimentally verified. In the third phase, a mathematical model was developed to describe the gravity-driven degradation of concentricity in molten glass shells.

Nolen, R. L.↗

Experimental methods for quenching structures in lunar-analog silicate melts: Variations as a function of quench media and composition

Compositions analogous to lunar green, organge, and brown glasses were synthesized under consistent conditions, then quenched into a variety of different media when the samples were removed from the furnace. Iron valence and coordination are a direct function of quench media used, spanning the range from brine/ice (most effective quench), water, butyl phthalate, silicone oil, liquid nitrogen, highly reducing CO-CO2 gas, to air (least efficient quench). In the green and brown glasses, Fe(3+) in four-fold and six-fold coordination is observed in the slowest-quenched samples; Fe(2+) coordination varies directly with quench efficiency. Less pronounced changes were observed in the Ti-rich orange glass. Therefore the remote-sensed spectrum of a glass-bearing regolith on the Moon may be influenced by the process by which the glass cooled, and extreme caution must be used when comparing spectra of synthetic glass analogs with real lunar glasses.

Dyar, M. D.↗

Experimental methods for quenching structures in lunar-analog silicate melts - Variations as a function of quench media and composition

Compositions analogous to lunar green, orange, and brown glasses were synthesized under consistent conditions, then quenched into a variety of different media when the samples were removed from the furnace. Iron valence and coordination are a direct function of quench media used, spanning the range from brine/ice (most effective quench), water, butyl phthalate, silicone oil, liquid nitrogen, highly reducing CO-CO2 gas, to air (least efficient quench). In the green and brown glasses, Fe(3+) in four-fold and six-fold coordination is observed in the slowest-quenched samples; Fe(2+) coordination varies directly with quench efficiency. Less pronounced changes were observed in the Ti-rich orange glass. Therefore the remote-sensed spectrum of a glass-bearing regolith on the moon may be influenced by the process by which the glass cooled, and extreme caution must be used when comparing spectra of synthetic glass analogs with real lunar glasses.

Dyar, M. D.↗

Space Station Furnace Facility - A multipurpose, high temperature microgravity research facility

This paper describes the Space Station Furnace Facility (SSFF) program. The SSFF is a new development intended to provide an advanced facility for materials research in the microgravity environment of the Space Station. The SSFF will be designed for research in metals, oxides, glasses, and alloy solidification and crystal growth of electronic and electrooptical materials. The facility will be designed to process multiple samples in one or more furnaces in an automated mode. The SSFF will be built around a general facility core which will provide common support functions not provided by the Space Station, subsystems which could best be centralized, and common subsystems which could be distributed with each experiment module. The SSFF will be capable of operation in both the manned and unmanned mode and is scheduled for early deployment aboard the Space Station.

Kirkindall, Arthur S.↗

Containerless Processing of a Lithium Disilicate Glass

Glasses of Li2O.2SiO2 (LS2), and LS2 doped with 0.001wt% platinum (LS2 + 0.001 wt% Pt) compositions were melted, cooled and reheated at controlled rates while levitated (containerless) inside an Electrostatic Levitator (ESL) furnace at the NASA Marshall Space Flight Center, Huntsville, AL. The experiments were conducted in vacuum (approximately 10(exp -5) Pa) using spherical, 2.5 to 3 millimeter diameter, glass samples. The measured critical cooling rate for glass formation, R(sub c), for the LS2 and LS2+0.001 wt% Pt glasses processed at ESL were 14 plus or minus 2 Celsius per minute and 130 plus or minus 5 Celsius per minute, respectively. The values of R(sub c), for the same LS2 and LS2 + 0.001 wt% Pt glasses processed in a container were 62 plus or minus 3 Celsius per minute and 162 plus or minus 5 Celsius per minute, respectively. The effective activation energy for crystallization, E, for this LS2 glass processed without a container at ESL, 392 plus or minus 15 kiloJoules per mole, was higher than that, 270 plus or minus 15 kiloJoules per mole, for an identical glass processed in a container. These results suggest that the glass formation tendency for a containerless LS2 melt is significantly increased compared to an identical melt in contact with a container. The absence of heterogeneous nucleation sites that are inherently present in all melts held in containers, and or a change in the surface composition due to evaporation of Li2O during processing at ESL are likely reasons for the increased glass forming tendency of this containerless LS2 melt.

Ranasinghe, Kisa↗

High waste loading glass formulation development for high-P HLW

The primary objective of the work described herein was to develop and identify HLW glass compositions and glass forming additive blends that achieve high waste loadings and processing rates for high phosphorus HLW streams while maintaining acceptable glass properties. This was accomplished through a combination of crucible-scale tests, vertical gradient furnace tests, and confirmation tests on the DM100 melter system.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Containerless high purity pulling process and apparatus for glass fiber

Apparatus and method for pulling optical glass fibers in a containerless environment is disclosed which includes a single axis acoustical levitation furnace in which a specimen is levitated and melted. A reflector unit is carried in the interior of the furnace and includes a reflector disposed centrally about the acoustical axis of the levitator. The reflector unit includes a circular shroud of insulation and a copper sleeve inserted in the unit which is hollow at for receiving a cooling medium. A fiber pulling bore is formed centrally in the reflector unit surrounded by cooling jacket to enhance solidification and formation of a fiber. A starting fiber strand is introduced into the melt and pulled outwardly through bore whereby the specimen fiber is started and formed as pulled therethrough. In order to replenish the melt and thus enable a continous process, a movable secondary reflector is provided which captures a supplemental specimen pellet and by movement of the reflector transfers it to the melt.

Naumann, R. J.↗

Investigation of microgravity effects on solidification phenomena of selected materials

A Get Away Special (GAS) experiment payload to investigate microgravity effects on solidification phenomena of selected experimental samples has been designed for flight. It is intended that the first flight of the assembly will (1) study the p-n junction characteristics for advancing semiconductor device applications, (2) study the effects of gravity-driven convection on the growth of HgCd crystals, (3) compare the textures of the sample which crystallizes in microgravity with those found in chondrite meteorites, and (4) modify glass optical characteristics through divalent oxygen exchange. The space flight experiment consists of many small furnaces. While the experiment payload is in the low gravity environment of orbital flight, the payload controller will sequentially activate the furnaces to heat samples to their melt state and then allow cooling to resolidification in a controlled fashion. The materials processed in the microgravity environment of space will be compared to the same materials processed on earth in a one-gravity environment. This paper discusses the design of all subassemblies (furnance, electronics, and power systems) in the experiment. A complete description of the experimental materials is also presented.

Maag, Carl R.↗

Alkali Vapor Corrosion of Spinel (MgAl 2 O 4 ) and Gahnite (ZnAl 2 O 4 ) Refractories—A Comparative Study

Alkali vapor corrosion is critical for refractories used in the kilns and furnaces of diverse high-temperature processing and manufacturing sectors such as gasifiers, cement production, and glass making. Gahnite (ZnAl 2 O 4 ) is being investigated as a potential chrome-free refractory because of its similarity with the structure and properties of magnesium aluminate (MgAl 2 O 4 ) spinel. The alkali vapor corrosion of ZnAl 2 O 4 , MgAl 2 O 4 , and Mg 0.5 Zn 0.5 Al 2 O 4 was studied, according to ASTM C987-10, at 1371°C for 24 h using sodium carbonate (Na 2 CO 3 ). The surface and the polished cross-sections of the corroded ZnAl 2 O 4 , MgAl 2 O 4 , and Mg 0.5 Zn 0.5 Al 2 O 4 specimens were analyzed using x-ray diffraction (XRD), microscopy, and energy-dispersive spectroscopy (EDS) techniques. MgO in MgAl 2 O 4 , ZnO in ZnAl 2 O 4 , Mg 0.77 Zn 0.23 O, and NaAlO 2 were detected as the corrosion products for these specimens. The extent of corrosion substantially varied among the specimens despite the similarity in the corrosion products. The corrosion resistance increased in the following order: Mg 0.5 Zn 0.5 Al 2 O 4 > MgAl 2 O 4 > ZnAl 2 O 4 . The formation of a dense MgO and Mg 0.77 Zn 0.23 O layer for MgAl 2 O 4 and Mg 0.5 Zn 0.5 Al 2 O 4 , respectively, contributed to their superior resistance to alkali vapor corrosion. The underlying corrosion mechanisms are discussed based on experimental observations supported by thermodynamic analysis. Additionally, the results suggest that a partial Zn 2+ substitution for Mg 2+ in MgAl 2 O 4 can enhance the resistance to alkali vapor corrosion.

alkali corrosion↗

Simple device measures solar radiation

Simple inexpensive thermometer, insolated from surroundings by transparent glass or plastic encasement, measures intensities of solar radiation, or radiation from other sources such as furnaces or ovens. Unit can be further modified to accomplish readings from remote locations.

Humphries, W. R.↗

Extraterrestrial fiberglass production using solar energy

A conceptual design is presented for fiberglass production systems in both lunar and space environments. The raw material, of lunar origin, will be plagioclase concentrate, high silica content slag, and calcium oxide. Glass will be melted by solar energy. The multifurnace in the lunar plant and the spinning cylinder in the space plant are unique design features. Furnace design appears to be the most critical element in optimizing system performance. A conservative estimate of the total power generated by solar concentrators is 1880 kW; the mass of both plants is 120 tons. The systems will reproduce about 90 times their total mass in fiberglass in 1 year. A new design concept would be necessary if glass rods were produced in space.

Ho, D.↗

Crystallization of baria-titania-silica glasses

The critical cooling rate for glass formation, Rc, and the crystallization kinetics of the compositions (1/2)(100-x)BaO-(1/2)(100-x)TiO2-(x)SiO2 with x = 20, 25, 30, 33.3, and 40 mol pct were studied using a thermal image furnace. Crystallization was studied under nonisothermal conditions, and the data were analyzed using the Johnson-Mehl-Avrami equation. The Rc and activation energy for crystallization both decrease with increasing silica content. Fresnoite, Ba2TiSi2O8, crystallized from all of the glasses when they were reheated. The infrared absorption spectra of the glasses and crystals show that they both contain (Si2O7) and square pyramidal (TiO5) groups.

Ray, Chandra S.↗

Acoustic positioning for space processing experiments

An acoustic positioning system is described that is adaptable to a range of processing chambers and furnace systems. Operation at temperatures exceeding 1000 C is demonstrated in experiments involving the levitation of liquid and solid glass materials up to several ounces in weight. The system consists of a single source of sound that is beamed at a reflecting surface placed a distance away. Stable levitation is achieved at a succession of discrete energy minima contained throughout the volume between the reflector and the sound source. Several specimens can be handled at one time. Metal discs up to 3 inches in diameter can be levitated, solid spheres of dense material up to 0.75 inches diameter, and liquids can be freely suspended in l-g in the form of near-spherical droplets up to 0.25 inch diameter, or flattened liquid discs up to 0.6 inches diameter. Larger specimens may be handled by increasing the size of the sound source or by reducing the sound frequency.

Whymark, R. R.↗