New Mie Scattering Diffuse Targets Development and Characterization
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Bidirectional Reflectance Distribution Function↗
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Monte Carlo Simulation of Nanoparticle Encapsulation in Flames
Gas-phase combustion (flame) synthesis has been an essential industrial process for producing large quantities of powder materials such as carbon black, titanium dioxide, and silicon dioxide. Flames typically produce simple oxides, with carbon black being the noted exception because the oxides of carbon are gaseous and are easily separated from the particulate matter that is formed during fuel pyrolysis. Furthermore, the powders produced in flames are usually agglomerated, nanometer-sized particles (nanoparticles). This composition and morphology is acceptable for many applications. However, the present interest in nanoparticles for advanced materials application has led to efforts to employ flames for the synthesis of unagglomerated nanoparticles (2 to 100 nm) of metals and non-oxide ceramics. Sodium-halide chemistry has proven to be viable for producing metals and non-oxide ceramics in flames. Materials that have been produced to date include Si (Calcote and Felder, 1993), TiN, TiB2, TiC, TiSi2, SiC, B4C (Glassman et al, 1993) Al, W, Ti, TiB2, AlN, and W-Ti and Al-AlN composites (DuFaux and Axelbaum, 1995, Axelbaum et al 1996,1997). Many more materials are possible. The main challenge that faces application of flame synthesis for advanced materials is overcoming formation of agglomerates in flames (Brezinsky, 1997). The high temperatures and high number densities in the flame environment favor the formation of agglomerates. Agglomerates must be avoided for many reasons. For example, when nanopowders are consolidated, agglomerates have a deleterious effect on compaction density, leading to voids in the final part. Efforts to avoid agglomeration in flames without substantially reducing particle number density and, consequently, production rate, have had limited success. Another critical challenge that faces all synthesis routes for nanopowders is ensuring that the powders are high purity and that the process is scaleable. Though the containerless, high temperature environment of a flame is excellent for producing high-purity simple compounds, ultrafine metals and non-oxide ceramic powders are inherently reactive in the presence of oxygen and/or moisture. Thus, the handling of these powders after synthesis poses a challenging problem. Impurities acquired during handling of nanoparticles have plagued the advancement of nanostructured materials technology.
Sun, Z.↗
Understanding Binder–Silicon Interactions during Slurry Processing
The conformation of poly(acrylic acid) (PAA) as a function of shear during slurry processing to construct silicon-based anodes is elucidated via rheology-coupled ultra-small-angle neutron scattering (rheo-USANS). Rheo-USANS shows that PAA with encapsulated silicon exists as discrete aggregates that do not interact with one another. As a result, a well-connected matrix of silicon and carbon black dispersed in PAA does not exist; thus, the electrode is inhomogeneous. Raman mapping and X-ray photoelectron spectroscopy were used to confirm the electrode heterogeneity and further understand the cycling properties. These results are correlated to silicon surface chemistry to provide a pathway to making better electrodes.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Orbital atomic oxygen effects on thermal control and optical materials - STS-8 results
The effects of exposing 23 specimens of optical and thermal control materials to space at 120 km altitude for over 40 hrs during the STS-8 mission are discussed. Ten samples of paint targeted for the Space Telescope (ST) and the Tethered Satellite were exposed, and included polyurethane, oxide, silicone, and glossy black and white samples which were scanned for alterations in the optical properties after being retrieved. Nine mirror-type materials were also investigated, along with silver specimens typical of solar cell interconnects. The oxygen flow at the orbital altitude was 3.5 x 10 to the 20th atoms/cu cm. The exposures caused no degradation of the magnesium fluoride mirror coatings, while the Kapton coating for the ST solar cell panels showed evidence of losing thickness. The Ag solar cell contacts will require coatings to extend their lifetimes. Overcoatings were also proven necessary for inhibiting degradation of painted surfaces.
Whitaker, A. F.↗
Spectral reflectance properties of carbon-bearing materials
The 0.3-2.6 micrometers spectral reflectance properties of carbon polymorphs (graphite, carbon black, diamond), carbides (silicon carbide, cementite), and macromolecular organic-bearing materials (coal, coal tar extract, oil sand, oil shale) are found to vary from sample to sample and among groups. The carbon polymorphs are readily distinguishable on the basis of their visible-near infrared spectral slopes and shapes. The spectra of macromolecular organic-bearing materials show increases in reflectance toward longer wavelengths, exceeding the reflectance rise of more carbon-rich materials. Reflectance spectra of carbonaceous materials are affected by the crystal structure, composition, and degree of order/disorder of the samples. The characteristic spectral properties can potentially be exploited to identify individual carbonaceous grains in meteorites (as separates or in situ) or to conduct remote sensing geothermometry and identification of carbonaceous phases on asteroids.
Cloutis, Edward A.↗
Investigation of the detectivity of radiation- produced defect levels in n and p type silicon and germanium Semiannual progress report
Black body responsivity data of n-type and p-type silicon
Mattauch, R. J.↗
Single crystal silicon filaments fabricated in SOI: A potential IR source for a microfabricated photometric CO2 sensor
The objective of this project was to design, fabricate, and test single crystal silicon filaments as potential black body IR sources for a spectrophotometric CO2 sensing microsystem. The design and fabrication of the silicon-on-insulator (SOI) filaments are summarized and figures showing the composite layout of the filament die (which contains four filaments of different lengths -- 500 microns, 1 mm, 1.5 mm and 2 mm -- and equal widths of 15 microns) are presented. The composite includes four mask layers: (1) silicon - defines the filament dimensions and contact pads; (2) release pit - defines the oxide removed from under the filament and hence, the length of the released filament; (3) Pyrex pit - defines the pit etched in the Pyrex cap (not used); and (4) metal - defines a metal pattern on the contact pads or used as a contact hole etch. I/V characteristics testing of the fabricated SOI filaments is described along with the nitride-coating procedures carried out to prevent oxidation and resistance instability.
Tu, Juliana↗
High and Ultra-High Temperature Reaction Kinetics by Single Nanoparticle Mass Spectrometry
Methodology is presented for non-destructive, optically-detected single nanoparticle (NP) mass spectrometry, with the goal of extracting surface reaction kinetics for single NPs at high temperatures. Methods for determining the NP charge, mass, and temperature as a function of time are discussed, and the data are used to extract both the absolute kinetics for mass change, as well as the efficiencies of the surface processes that cause them. Factors that contribute to the uncertainties in absolute and relative mass determination, and in the resulting kinetic parameters, are discussed. The method allows the NP-to-NP variations in initial reactivity to be measured directly, along with the time evolution of reactivity resulting from NP structural/compositional changes that occur under reaction conditions. The strengths and limitations of single nanoparticle mass spectrometry as a high temperature surface kinetics tool are discussed in the context of sublimation and O2 oxidation kinetics experiments for single hafnium (Hf) NPs at temperatures ranging above 2400 K. The Hf oxidation kinetics are compared to analogous oxidation experiments for silicon, graphite, and carbon black NPs. In all four cases, the oxidation chemistry was dominated by processes that result in net mass loss, and the distinct mechanisms responsible are discussed. All four NPs also eventually passivated, i.e., the efficiencies for oxidative etching decreased by at least two orders of magnitude, relative to the initial efficiencies. Furthermore, the passivation mechanisms, which are quite different for carbon, compared to silicon or hafnium, are discussed. Carbon NP passivation is attributed to structural isomerization leading to fully coordinated, fullerene-like NP surfaces, while for silicon and hafnium, passivation results from delayed formation of an oxide layer, triggered by accumulation of oxygen in the NP sub-surface region.
36 MATERIALS SCIENCE↗
Stability Enhancement of Polymeric Sensing Films Using Fillers
Experiments have shown the stability enhancement of polymeric sensing films on mixing the polymer with colloidal filler particles (submicron-sized) of carbon black, silver, titanium dioxide, and fumed silicon dioxide. The polymer films are candidates for potential use as sensing media in micro/nano chemical sensor devices. The need for stability enhancement of polymer sensing films arises because such films have been found to exhibit unpredictable changes in sensing activity over time, which could result in a possible failure of the sensor device. The changes in the physical properties of a polymer sensing film caused by the sorption of a target molecule can be measured by any of several established transduction techniques: electrochemical, optical, calorimetric, or piezoelectric, for example. The transduction technique used in the current polymer stability experiments is based on piezoelectric principles using a quartz-crystal microbalance (QCM). The surface of the QCM is coated with the polymer, and the mass uptake by the polymer film causes a change in the oscillating frequency of the quartz crystal. The polymer used for the current study is ethyl cellulose. The polymer/ polymer composite solutions were prepared in 1,3 dioxolane solvent. The filler concentration was fixed at 10 weight percent for the composites. The polymer or polymer composite solutions were cast on the quartz crystal having a fundamental frequency of about 6 MHz. The coated crystal was subjected to a multistage drying process to remove all measurable traces of the solvent. In each experiment, the frequency of oscillation was measured while the QCM was exposed to clean, dry, flowing air for about 30 minutes, then to air containing a known concentration of isopropanol for about 30 minutes, then again to clean dry air for about 30 minutes, and so forth. This cycle of measurements for varying isopropanol concentrations was repeated at intervals for several months. The figure depicts some of the sensing film stability results for ethyl cellulose polymer, ethyl cellulose-carbon black, and ethyl cellulose-silicon dioxide composite systems. An ethyl cellulose film exhibited a marked decline in response in the first few months of study and settled to a steady average response after about four months. However, response varied widely around the average response for ethyl cellulose film. In contrast, ethyl cellulose- carbon black and ethyl cellulose-silicon dioxide composites also declined in the early months, but showed more repeatable sensing film activity after the initial decline. Similar trends were observed in experiments for ethyl cellulose-titanium dioxide and ethyl cellulose-silver composites.
Lin, Brian↗
Using Optically Stimulated Electron Emission as an Inspection Method to Monitor Surface Contamination
During redesign of the Space Shuttle reusable solid rocket motor (RSRM), NASA amended the contract with ATK Launch Systems (then Morton Thiokol Inc.) with Change Order 966 to implement a contamination control and cleanliness verification method. The change order required: (1) A quantitative inspection method (2) A written record of actual contamination levels versus a known reject level (3) A method that is more sensitive than existing methods of visual and black light inspection. Black light inspection is only useful for inspection of contaminants that fluoresce near the 365 nm spectral line and is not useful for inspection of most silicones that will not produce strong fluorescence. Black light inspection conducted by a qualified inspector under controlled light is capable of detecting Conoco HD-2 grease in gross amounts and is very subjective due to operator sensitivity. Optically stimulated electron emission (OSEE), developed at the Materials and Process Laboratory at Marshall Space Flight Center (MSFC), was selected to satisfy Change Order 966. OSEE offers several important advantages over existing laboratory methods with similar sensitivity, e.g., spectroscopy and nonvolatile residue sampling, which provide turn around time, real time capability, and full coverage inspection capability. Laboratory methods require sample gathering and in-lab analysis, which sometimes takes several days to get results. This is not practical in a production environment. In addition, these methods do not offer full coverage inspection of the large components
Lingbloom, Mike S.↗
An overview of the first results on the solar array passive LDEF experiment (sample), AO171
Space environmental effects were visibly obvious on components of experiment AO171 which contained solar cells, composites, polymeric thin films, solar reflectors, protective coatings, metals, paints , and elastomers. Micrometeoroid/space debris impacts were observed on all experiment elements. Luminescence of polyimide, silicone, and polyurethane materials occurred under black light examination. Outgassing of RTV511 occurred mainly as a result of insufficient thermal vacuum bakeout. Solar cell degradation was predominantly below 10 percent. Elastomers lost mass and discolored; composites showed evidence of atomic oxygen attack, and unprotected thin polymer films eroded away.
Whitaker, Ann F.↗
Follow-up on the effects of the space environment on UHCRE thermal blankets
An overview of the effects of the space environment on the thermal blanket of the UHCRE experiment is presented with an emphasis on atomic oxygen (AO) erosion. A more accurate value for FEP Teflon reaction efficiency is given and corresponds, at normal incidence, to 3.24 10(exp -25) cu cm/atomic, therefore, the FEP Teflon erosion corresponding to the Long Duration Exposure Facility (LDEF) total mission is 29.5 microns. A power 1.44 of the cosine of the incident angle of the oxygen atoms is found. It is shown that this value is not far from the power found using Fergusson's relationship between efficiency and energy of the O-atoms. An hypothesis concerning the effect of oxygen ions (O(+)) is also presented. The presence of oxygen ions may explain the different results obtained from different flights and from laboratory tests. Finally an XPS analysis of Chemglaze Z306(tm) black paint demonstrates the presence of silicone in the paint which may explain part of the contamination found on LDEF.
Levadou, Francois↗
Light-weight ceramic insulation
Ultra-high temperature, light-weight, ceramic insulation such as ceramic tile is obtained by pyrolyzing a siloxane gel derived from the reaction of at least one organo dialkoxy silane and at least one tetralkoxy silane in an acid or base liquid medium. The reaction mixture of the tetra- and dialkoxy silanes may contain also an effective amount of a mono- or trialkoxy silane to obtain the siloxane gel. The siloxane gel is dried at ambient pressures to form a siloxane ceramic precursor without significant shrinkage. The siloxane ceramic precursor is subsequently pyrolyzed, in an inert atmosphere, to form the black ceramic insulation comprising atoms of silicon, carbon and oxygen. The ceramic insulation, can be characterized as a porous, uniform ceramic tile resistant to oxidation at temperatures ranging as high as 1700.degree. C. and is particularly useful as lightweight tiles for spacecraft and other high-temperature insulation applications.
Hsu, Ming-Ta S.↗
Light-weight black ceramic insulation
Ultra-high temperature, light-weight, black ceramic insulation having a density ranging from about 0.12 g/cc. to 0.6 g/cc. such as ceramic tile is obtained by pyrolyzing siloxane gels derived from the reaction of at least one organo dialkoxy silane and at least one tetralkoxy silane in an acid or base liquid medium. The reaction mixture of the tetra- and dialkoxy silanes also may contain an effective amount of a mono- or trialkoxy silane to obtain the siloxane gels. The siloxane gels are dried at ambient temperatures and pressures to form siloxane ceramic precursors without significant shrinkage. The siloxane ceramic precursors are subsequently pyrolyzed, in an inert atmosphere, to form the black ceramic insulation comprising atoms of silicon, carbon and oxygen. The ceramic insulation can be characterized as a porous, uniform ceramic tile resistant to oxidation at temperatures ranging as high as 1700.degree. C., and particularly useful as lightweight tiles for spacecraft and other high-temperature insulation applications.
Hsu, Ming-Ta S.↗
An Optical Oxygen Sensor for Long-Term Continuous Monitoring of Dissolved Oxygen in Perfused Bioreactors
For long-term growth of man1ITlalian cells in perfused bioreactors, it is essential to monitor the concentration of dissolved oxygen (DO) present in the culture medium to quantitate and control level of DO. Continuous measurement of the amount of DO in the cell culture medium in-line under sterile conditions in NASA's perfused bioreactor requires that the oxygen sensor provide increased sensitivity and be sterilizable and nontoxic. Additionally, long-term cell culture experiments require that the calibration be maintained several weeks or months. Although there are a number of sensors for dissolved oxygen on the market and under development elsewhere, very few meet these stringent conditions. An optical oxygen sensor (BOXY) based on dynamic fluorescent quenching and a pulsed blue LED light source was developed in our laboratory to address these requirements. Tris( 4,7 -diphenyl-l, 1 O-phenanthroline )ruthenium(II) chloride is employed as the fluorescent dye indicator. The sensing element consists of a glass capillary (OD 4.0 mm; ID 2.0 mm) coated internally with a thin layer of the fluorescent dye in silicone matrix and overlayed with a black shielding layer. Irradiation of the sensing element with blue light (blue LED with emission maximum at 475 nm) generates a red fluorescence centered at 626 nm. The fluorescence intensity is correlated to the concentration of DO present in the culture medium, following the modified non-linear Stern-Volmer equation. By using a pulsed irradiating light source, the problem of dye-bleaching, which is often encountered in long-term continuous measurements of tIns type, 'is minimized. To date we achieved sensor resolution of 0.3 mmHg at 50 mmHg p02, and 0.6 mmHg at 100 mmHg p02, with a response time of about one minute. Calibration was accomplished in sterile phosphate-buffered saline with a blood-gas analyzer (BGA) measurement as reference. Stand-alone software was also developed to control the sensor and bioreactor as well as to acquire data. Two HOXY sensors with a single calibration were employed to continuously monitor the DO in GTSF-2 medium during a Baby Hamster Kidney (BHK-21) cell culture in a Rotating Wall Perfused Vessel (RWPV) bioreactor for 90 days. HOXY sensors were located at the inlet to and outlet from the bioreactor. One of the sensors was placed between an oxygenator and the inlet to the bioreactor. The dissolved oxygen concentrations determined by both sensors were compared with those measured regularly with the BGA reference. The cell culture was maintained for 110 days. Sensor output was found to correlate well with the BGA data throughout the experiment, where the DO of the medium ranged between 25 and 50 mmHg at the bioreactor outlet and 90-130 mmHg at the bioreactor inlet. Measuring DO with the HOXY sensors versus the BGA reference indicated bias values of -2 mmHg and -15 mmHg, and precision values of +/-3mmHg and +/-16 mmHg at the bioreactor inlet and outlet, respectively.
Gao, F. G.↗
Flouorescence measurements of the thermal control coatings on LDEF experiments S0069 and A0114
Strong fluorescence emissions were observed, during post flight ultraviolet light inspection of experiments S0069 and A0114, from some of the surfaces exposed to the space environment. Subsequent wavelength measurements of the fluorescence emission characteristics, indicated large changes occurred between controls and exposed materials. Black urethane based coatings, especially ones having a silicone atomic oxygen protective overcoat, appear bright yellow under ultraviolet exposure. Measurements showed that the urethane based coatings had their emission spectra shifted into the visible wavelength range. In contrast, zinc oxide pigment type coatings showed a different effect, which was a quenching or reduction of their fluorescence versus exposure time. Silver Teflon bonded to aluminum with acrylic adhesive also showed a slight measurable fluorescence, which was found to originate in the acrylic adhesive.
Zwiener, James M.↗
Development of material specifications and qualifications of polymeric materials for the jpl spacecraft materials guidebook. ii- rtv silicone adhesives and potting compounds special report no. 2
Silicone rubber adhesives and potting compounds - polymeric materials for spacecraft
POTTING COMPOUND↗
Nanostructure Secondary-Mirror Apodizing Mask for Transmitter Signal Suppression in a Duplex Telescope
A document discusses a nanostructure apodizing mask, made of multi-walled carbon nanotubes, that is applied to the centers (or in and around the holes) of the secondary mirrors of telescopes that are used to interferometrically measure the strain of space-time in response to gravitational waves. The shape of this ultra-black mask can be adjusted to provide a smooth transition to the clear aperture of the secondary mirror to minimize diffracted light. Carbon nanotubes grown on silicon are a viable telescope mirror substrate, and can absorb significantly more light than other black treatments. The hemispherical reflectance of multi-walled carbon nanotubes grown at GSFC is approximately 3 to 10 times better than a standard aerospace paint used for stray light control. At the LISA (Laser Interferometer Space Antenna) wavelength of 1 micron, the advantage over paint is a factor of 10. Primarily, in the center of the secondary mirror (in the region of central obscuration, where no received light is lost) a black mask is applied to absorb transmitted light that could be reflected back into the receiver. In the LISA telescope, this is in the center couple of millimeters. The shape of this absorber is critical to suppress diffraction at the edge. By using the correct shape, the stray light can be reduced by approximately 10 to the 9 orders of magnitude versus no center mask. The effect of the nanotubes has been simulated in a stray-light model. The effect of the apodizing mask has been simulated in a near-field diffraction model. Specifications are geometry-dependent, but the baseline design for the LISA telescope has been modeled as well. The coatings are somewhat fragile, but work is continuing to enhance adhesion.
Hagopian, John↗