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At least 1,297 records · Page 72

Material processing of convection-driven flow field and temperature distribution under oblique gravity

A set of mathematical formulation is adopted to study vapor deposition from source materials driven by heat transfer process under normal and oblique directions of gravitational acceleration with extremely low pressure environment of 10(exp -2) mm Hg. A series of time animation of the initiation and development of flow and temperature profiles during the course of vapor deposition has been obtained through the numerical computation. Computations show that the process of vapor deposition has been accomplished by the transfer of vapor through a fairly complicated flow pattern of recirculation under normal direction gravitational acceleration. It is obvious that there is no way to produce a homogeneous thin crystalline films with fine grains under such a complicated flow pattern of recirculation with a non-uniform temperature distribution under normal direction gravitational acceleration. There is no vapor deposition due to a stably stratified medium without convection for reverse normal direction gravitational acceleration. Vapor deposition under oblique direction gravitational acceleration introduces a reduced gravitational acceleration in vertical direction which is favorable to produce a homogeneous thin crystalline films. However, oblique direction gravitational acceleration also induces an unfavorable gravitational acceleration along horizontal direction which is responsible to initiate a complicated flow pattern of recirculation. In other words, it is necessary to carry out vapor deposition under a reduced gravity in the future space shuttle experiments with extremely low pressure environment to process vapor deposition with a homogeneous crystalline films with fine grains. Fluid mechanics simulation can be used as a tool to suggest most optimistic way of experiment with best setup to achieve the goal of processing best nonlinear optical materials.

Hung, R. J.↗

Diacetylene and Polydiacetylene Derivatives of 2-Methyl-4-Nitroaniline for Second-Harmonic Generation

A novel diacetylene derivative of 2-Methyl-4-NitroAniline (MNA), a well-known material for Second-Harmonic Generation (SHG), is synthesized. This monomer DiAcetylene MethylNitroAniline, (DAMNA) is characterized by means of the Kurtz technique at 1064 nm and is found to have an SHG powder efficiency 62.5 % that of MNA itself. Thin crystalline films of DAMNA are grown onto quartz, Teflon, and Kapton substrates by means of vapor deposition in vacuum. These films are then polymerized in the solid state by exposure to long-wavelength UV radiation to give crystalline polydiacetylene thin films (PDAMNA). The films are next characterized for SHG, using an unpolymerized DAMNA film as a reference. Interestingly, films grown onto Teflon exhibit greater orientation and significantly greater SHG than those grown onto quartz and Kapton. This result is promising in that it demonstrates the potential of PDAMNA as both a crystalline and polymeric material for SHG applications, in which highly oriented thin films are desired. Computational modeling (usingAM1) is also carried out on DAMNA and is compared to the experimental results.

Paley, M. S.↗

Soot Precursor Material: Visualization Via Simultaneous LIF-LII and Characterization Via TEM

Simultaneous combined laser-induced fluorescence and laser-induced incandescence (LIF-LII) images are presented for both a normal and inverse diffusion flame. The excitation wavelength dependence distinguishes the LIF and LII signals in images from the normal diffusion flame while the temporal decay distinguishes the signals in images of the inverse diffusion flame. Each flame presents a minimum in the combined LIF-LII intensity in a region separating the fuel pyrolysis and soot containing regions. Opacity, geometric in definition, and extent of crystallinity measured through both bright and dark field Transmission Electron Microscopy (TEM) characterizes the thermophoretically sampled material from within this minimal LIF-LII intensity region. TEM analysis reveals rather different soot processes occurring within the normal and inverse diffusion flame. In the normal diffusion flame, rapid chemical and physical coalescence of PAHs results in initial formation of soot precursor particles that are highly crystalline and evolve toward fully formed soot. In the inverse diffusion flame, rapid coalescence of pyrolysis products occurs, producing tarlike, globular structures equivalent in size to fully formed soot aggregates but with markedly less crystallinity than normal-appearing soot. These different material properties are interpreted as reflecting different relative rates of chemical and physical coalescence of fuel pyrolysis products versus carbonization. Significantly, these TEM images support qualitative photophysical arguments suggesting that, in general, this 'dark' region observed in the LIF-LII images demarcates a transitional region in which a fundamental change in the material the material chemical/physical properties occurs between solid carbonaceous soot and condensed or gaseous molecular growth material.

VanderWal, Randall L.↗

Chemical and Thermal Analysis

Work during the past three years has included significant research in several areas aimed at further clarification of the aging and chemical failure mechanism of thermoplastics (PVDF or Tefzel) for pipes. Among the areas investigated were the crystallinity changes associated with both the Coflon and Tefzel after various simulated environmental exposures using X-Ray diffraction analysis. We have found that significant changes in polymer crystallinity levels occur as a function of the exposures. These crystallinity changes may have important consequences on the fracture, fatigue, tensile, and chemical resistance of the materials. We have also noted changes in the molecular weight distribution and the increased crosslinking of the Coflon material using Gel Permeation Chromatographic Analysis. Again these changes may result in variations in the mechanical and chemical properties in the material. We conducted numerous analytical studies with methods including X-ray Diffraction, Gel Permeation Chromatography, Fourier Transform Infrared Spectroscopy, and Differential Scanning Calorimetry. We investigated a plethora of aged samples of both Tefzel and Coflon that were forwarded from MERL. Pressurized tests were performed on powdered PVDF in a modified Fluid A, which we will call A-2. In this case the ethylene diamine concentration was increased to 3 percent in methanol. Coflon pipe sections and powdered Coflon were exposed in pressure cells at 1700 psi at three separate test temperatures.

Bulluck, J. W.↗

Chemical and Thermal Analysis

Work has included significant research in several areas aimed at further clarification of the aging and chemical failure mechanism of thermoplastics (PVDF or Tefzel) for pipes. Among the areas investigated were the crystallinity changes associated with both the Coflon and Tefzel after various simulated environmental exposures using X-Ray diffraction analysis. We have found that significant changes in polymer crystallinity levels occur as a function of the exposures. These crystallinity changes may have important consequences on the fracture, fatigue, tensile, and chemical resistance of the materials. We have also noted changes in the molecular weight distribution of the Coflon material using a dual detector Gel Permeation Analysis. Again these changes may result in variation in the mechanical and chemical properties in the material. We conducted numerous analytical studies with methods including X-Ray Diffraction, Gel Permeation Chromatography, Fourier Transform Infrared Spectroscopy, Thermogravimetric Analysis, and Differential Scanning Calorimetry. We investigated a number of aged samples of both Tefzel and Coflon that were forwarded from MERL. Pressurized tests were performed in a modified Fluid G, which we will call G2. In this case the ethylene diamine concentration was increased to 3 percent in methanol. Coflon pipe sections and powdered Coflon were exposed in pressure cells at 1700 psi at three separate test temperatures, 70 C, 110 C, and 130 C. The primary purpose of the pressure tests in Fluid G2 was to further elucidate the aging mechanism of PVDF degradation.

Bulluck, J. W.↗

International Research Project on the Effects of Chemical Ageing of Polymers on Performance Properties: Chemical and Thermal Analysis

Work during the past six months has included significant research in several areas aimed at further clarification of the aging and chemical failure mechanism of thermoplastics (PVDF or Tefzel) pipes. Among the areas investigated were the crystallinity changes associated with both the Coflon and Tefzel after various simulated environmental exposures using X-ray diffraction analysis. We have found that significant changes in polymer crystallinity levels occur as a function of the exposures. These crystallinity changes may have important consequences on the fracture, fatigue, tensile, and chemical resistance of the materials. We have also noted small changes in the molecular weight distribution. Again these changes may result in variations in the mechanical and chemical properties in the material. We conducted numerous analytical studies with methods including X-ray Diffraction, Gel Permeation Chromatography, Fourier Transform Infrared Spectroscopy, Ultra- Violet Scanning Analysis, GC/Mass Spectrometry, Differential Scanning Calorimetry and Thermomechanical Analysis. In the ultra-violet analysis we noted the presence of an absorption band indicative of triene formation. We investigated a number of aged samples of both Tefzel and Coflon that were forwarded from MERL. We also cast films at SWT and subjected these films to a refluxing methanol 1% ethylene diamine solution. An updated literature search was conducted using Dialog and DROLLS to identify any new papers that may have been published in the open literature since the start of this project. The updated literature search and abstracts are contained in the Appendix section of this report.

Bulluck, J. W.↗

Space Weathering in the Fine Size Fractions of Lunar Soils: Soil Maturity Effects

The effects of space weathering on the optical properties of lunar materials have been well documented. These effects include a reddened continuum slope, lowered albedo, and attenuated absorption features in reflectance spectra of lunar soils as compared to finely comminuted rocks from the same Apollo sites. However, the regolith processes that cause these effects are not well known, nor is the petrographic setting of the products of these processes fully understood. A Lunar Soil Characterization Consortium has been formed with the purpose of systematically integrating chemical and mineralogical data with the optical properties of lunar soils. Understanding space-weathering effects is critical in order to fully integrate the lunar sample collection with remotely-sensed data from recent robotic missions (e.g., Lunar Prospector, Clementine, and Galileo) We have shown that depositional processes (condensation of impact-derived vapors, sputter deposits, accreted impact material, e.g., splash glass, spherules, etc.) are a major factor in the modification of the optical surfaces of lunar regolith materials. In mature soils, it is the size and distribution of the nanophase metal in the soil grains that has the major effect on optical properties. In this report, we compare and contrast the space-weathering effects in an immature and a mature soil with similar elemental compositions. For this study, we analyzed <10 micron sieve fractions of two Apollo 17 soils, 79221 (mature, Is/FeO = 81) and 71061 (immature, Is/FeO = 14). Details of the sieving procedures and allocation scheme are given else where. The results of other detailed chemical, mineralogical, and spectroscopic analyses of these soil samples are reported elsewhere. A representative sample of each soil was embedded in low-viscosity epoxy, and thin sections (about 70nm thick) were obtained through ultra microtomy. The thin sections used for these analyses typically contained cross sections of up to 500 individual grains. The thin sections were studied using a JEOL 2010 transmission electron microscope (TEM) equipped with a thin window energy-dispersive X-ray (EDX) spectrometer. An individual thin section was selected from each soil, and for each grain in the section we determined (1) the elemental composition by EDX; (2) whether the grain was crystalline or glassy using electron diffraction and darkfield imaging; (3) the presence or absence of rims and accreted material; and (4) the distribution of nanophase Fe where present. Most of the categories are self-evident; however, we divide the agglutinate derived material into agglutinitic glass (glass with approximately the same composition as the bulk soil that contains nanophase Fe with or without vesicles) and agglutinate fragments, which are composed of crystalline grains and agglutinitic glass. Lithic fragments are defined as polymineralic grains with no glass. Pyroxene grains have been divided into high- and low-Ca groups. As expected, there are a number of differences in the petrography of the <10-microns fractions of 79221 and 71061 given the great difference in their respective maturities, but we focus here on two major distinctions: agglutinate content and the number of grains with micropatina. Slightly over 50% of the particles in 79221 consist of agglutinitic glass and agglutinate fragments, while the remainder are predominantly crystalline mineral grains. The agglutinic glass particles contain abundant nanophase Fe and vesicles. Angular particles are rare, with most showing smooth, rounded exteriors, Of the mineral grains analyzed thus far, over 90% of the grains have amorphous rims that contain nanophase Fe (these rims are believed to have formed by vapor deposition and irradiation effects). The nanophase Fe in these rims probably accounts for a significant fraction of the increase in Is/FeO measured in these size fractions. In addition to the rims, the majority of particles also show abundant accreted material in the form of glass splashes and spherules that also contain nanophase Fe. In stark contrast, the surfaces of the mineral grains in the 71061 sample are relatively prisitine, as only about 14% of the mineral grains in the sample exhibited amorphous rims. Furthermore, the mineral particles are more angular and show greater surface roughness than in the mature sample. Accreted material on particle surfaces is rare. Agglutinitic material is a major component of the 71061 sample; however, nanophase Fe and vesicles are not as well developed as in the 79221 sample. It is now recognized that nanophase Fe is probably the main agent in modifying the optical properties of lunar soil grains. The most important result of this study is the observation that in the fine size fractions of mature soils, nearly every grain has nanophase Fe within 100 run of the particle surface. (Additional Information contained in original)

Keller, L. P.↗

Spectral Behavior of Hematite at Visible/Near Infrared and Midinfrared Wavelengths

The oxide mineral hematite alpha-Fe2O3) is present on Mars as evidenced by spectroscopy using visible/near infrared (VNIR) and midinfrared (MIR) wavelengths. The physical nature of this surficial hematite varies from fine-grained, crystalline red hematite (red-Hm) in certain martian bright regions, to coarser-grained, crystalline gray hematite (gray-Hm) in the Sinus Meridiani equatorial site discovered in the Mars Global Surveyor Thermal Emission Spectrometer (MGS-TES) data. The VNIR spectra require that the red hematite is present in amounts subordinate to a second ferric pigment, which accounts for the general shape and position of the martian ferric absorption edge. By analogy with palagonitic tephra and synthetic samples, the pigment is a nanophase ferric oxide, possibly nanophase hematite (np-Hm). The purpose of this abstract is to document the physicospectral properties of hematite in the VNIR (0.35 to 2.2 microns) and MIR (5 to 25 microns) with respect to the terms "nanophase" and "crystalline", "red" and "gray", and "fine-grained" and "coarse-grained". We will show that different "types" of hematite (no-, red-, and gray-Hm) have different spectral responses in the VNIR and MIR regions and that these differences are important for inferring the types of hematite and their relative proportions from remotely sensed spectra of Mars. Because hematite is an alteration product that forms through many different geologic processes, determination of the type of hematite provides important clues about the style and diversity of martian weathering processes.

Lane, Melissa D.↗

Spectral Behavior of Hematite at Visible/Near Infrared and Midinfrared Wavelengths

The oxide mineral hematite alpha-Fe2O3) is present on Mars as evidenced by spectroscopy using visible/near infrared (VNIR) and midinfrared (MIR) wavelengths. The physical nature of this surficial hematite varies from fine-grained, crystalline red hematite (red-Hm) in certain martian bright regions, to coarser-grained, crystalline gray hematite (gray-Hm) in the Sinus Meridiani equatorial site discovered in the Mars Global Surveyor Thermal Emission Spectrometer (MGS-TES) data. The VNIR spectra require that the red hematite is present in amounts subordinate to a second ferric pigment, which accounts for the general shape and position of the martian ferric absorption edge. By analogy with palagonitic tephra and synthetic samples, the pigment is a nanophase ferric oxide, possibly nanophase hematite (np-Hm). The purpose of this abstract is to document the physicospectral properties of hematite in the VNIR (0.35 to 2.2 mm) and MIR (5 to 25 mm) with respect to the terms "nanophase" and "crystalline", "red" and "gray", and "fine-grained" and "coarse-grained". We will show that different "types" of hematite (np-, red-, and gray-Hm) have different spectral responses in the VNIR and MIR regions and that these differences are important for inferring the types of hematite and their relative proportions from remotely sensed spectra of Mars. Because hematite is an alteration product that forms through many different geologic processes, determination of the type of hematite provides important clues about the style and diversity of martian weathering processes. Additional information is contained in the original extended abstract.

Lane, M. D.↗

Retrieval of Polar Stratospheric Cloud Microphysical Properties From Lidar Measurements: Dependence on Particle Shape Assumptions

Knowledge of particle sizes and number densities of polar stratospheric clouds (PSCs) is highly important, because they are critical parameters for the modeling of the ozone chemistry of the stratosphere. In situ measurements of PSC particles are rare. the main instrument for the accumulation of PSC data are lidar systems. Therefore the derivation of some microphysical properties of PSCS from the optical parameters measured by lidars would be highly beneficial for ozone research. Inversion of lidar data obtained in the presence of PSCs formed from crystalline particles type 11 and the various nitric acid tri Ydrrate (NAT) types cannot be easily accomplished, because a suitable scattering theory for small faceted crystals has not been readily available tip to now. As a consequence, the T-matrix method is commonly used for the interpretation of these PSC lidar data. Here the assumption is made that the optical properties of an ensemble of spheroids resemble those of crystalline PSCs, and microphysical properties of the PSC are inferred from the optical signatures of the PSC at two or more wavelengths. The problem with the T-matrix approach is that the assumption of spheroidal instead of faceted particles can lead to dramatically wrong results: Usually cloud particle properties are deduced from analysis of lidar profiles of backscatter ratio and depolarization ratio. The particle contribution to the backscatter ratio is given by the product of the particle number density and the backscattering cross section. The latter is proportional to the value of the particle's scattering phase function at 180 degrees scattering angle. At 180 degrees however, the phase functions of rough, faceted crystals and of spheroids with same maximum dimension differ by a factor of 6. From this it follows that for a PSC consisting of faceted crystals, the particle number density is underestimated by roughly the same factor if spheroidal particles are unrealistically assumed. We are currently developing a retrieval technique for determining the microphysical parameters of crystalline PSCs that takes into account the faceted shape of the PSC particles. This approach utilizes finite-difference time-domain (FDTD) calculations of particle optical properties. The accuracy and the free choice of the shape of the scattering particle make the FDTD technique a promising tool for the inversion of PSC lidar data. A first comparison of FDTD and T-matrix calculations will be presented.

Reichardt, Susanne↗

Grain Properties of Comet C/1995 O1 (Hale-Bopp) Deduced Through Computational Techniques

We present the computational analysis of the 7.6 - 13.2 micrometer infrared (IR) spectrophotometry (R approximately equal to 120) of comet C/1995 O1 (Hale-Bopp) in conjunction with concurrent observations which extend the spectral energy distribution from the near-infrared to far-infrared wavelengths. The observations include temporal epochs pre-perihelion, (1996 October UT and 1997 February UT), near perihelion (1997 April UT), and postperihelion (1997 June UT). Through the computational modeling of small amorphous carbon, and crystalline and amorphous silicate grains in Hale-Bopp's coma, we find that as the comet approached perihelion, the grain size distribution (the Hanner modified power law) steepened (N = 3.4 pre-perihelion, to N = 3.7 near and post-perihelion) along with an increase in the fractal porosity of larger (greater than 1 micrometer) grains. The peak of the grain size distribution remained constant (ap = 0.2 micrometer) at each epoch. We attribute the emergence of the 9.3 micrometer peak near perihelion to crystalline orthopyroxeno grains released from inside the nucleus. Crystalline silicates (olivine and orthopyroxene) make up about 30% (by mass) of the submicron sized (less than 1 micrometer) dust grains in Hale-Bopp's coma during each epoch.

Harker, David E.↗

Cometary Science After Hale-Bopp

Comets and the chondritic porous interplanetary dust particles (CP IDPs) that they shed in their comae are reservoirs of primitive solar nebula materials. The high porosity and fragility of cometary grains and CP IDPs, and anomalously high deuterium contents of pyroxene-rich CP IDPs imply these aggregate particles contain significant interstellar grain components. Spectrophotometry of comets at thermal IR wavelengths (3-40 microns) reveal the presence of a warm (near-IR) featureless emission modeled by amorphous carbon grains, and mid-IR and far-IR broad and narrow resonances modeled by chondritic (50% Fe and 50% Mg) amorphous and Mg-rich crystalline silicate minerals, respectively. Cometary amorphous silicate resonances are well matched by IR spectra of CP IDPs dominated by 0.1 micron spherules of Glass with Embedded Metal and Sulfides (GEMS) that are thought to be the interstellar Fe-bearing amorphous silicates produced in the cooling outflows of Asymptotic Giant Branch (AGB) stars. Acid-etched microtomed CP IDP samples, however, show that both the carbon phase (aliphatic) and the amorphous silicate phase (Mg-rich) are not optically absorbing while the embedded Fe nanoparticles make the IDPs dark. The CP IDPs suggest either significant processing has occurred in the ISM or that the AGB amorphous silicates have Mg-rich stoichiometry and possibly grew on Fe particle condensates. Cometary crystalline silicate resonances are well matched by IR spectra of laboratory submicron Mg-rich olivine crystals, [Mg(sub y),Fe(sub 1-y)]2SiO4 with y/ge0.85, and in the case of Hale-Bopp at r(sub h) less than or equal to approx. 1.5 AU, by Mg-rich pyroxene crystals, [Mg(sub x),Fe(sub 1-x)]SiO3 with x/ge0.85. While a fraction of AGB stardust (less than or equal to 15%) are Mg-rich crystals, this interstellar star dust component is insufficient to account for the deduced abundance of crystalline minerals in comet dust. An insufficient source of ISM Mg-rich crystals leads to the inference that Mg-rich crystals in comets may be hot, early solar nebula condensates that traveled large radial distances out to the comet-forming zone.

Wooden, Diane H.↗

Twinning, Epitaxy and Domain Switching in Ferroelastic Inclusion Compounds

Our research is in the area of solid-state organic chemistry, which lies at the interface between physical organic chemistry and materials science. We use crystalline solids as models to probe fundamental issues about physical processes, molecular interactions and chemical reactions that are important for fabrication, stabilization and application of technological materials. Much of our most recent work has focused on the phenomena of ferroelastic and ferroelectric domain switching, in which application of an external force or electric field to a crystal causes the molecules inside the crystal to reorient, in tandem, to a new orientational state. To better understand and control the domain switching process, we have designed and synthesized over twenty closely related, ferroelastic organic crystals. Our approach has been to use crystalline inclusion compounds, in which one molecule (the guest) is trapped within the crystalline framework of a second molecule (the host). By keeping the host constant and varying the proportions and kinds of guests, it has been possible to tailor these materials so that domain switching is rapid and reversible (which is desirable for high technology applications). Inclusion compounds therefore serve as powerful systems for understanding the specific molecular mechanisms that control domain switching.

Hollingsworth, Mark D.↗

Nanolayered Features of Collagen-like Peptides

We have been investigating collagen-like model oligopeptides as molecular bases for complex ordered biomimetic materials. The collagen-like molecules incorporate aspects of native collagen sequence and secondary structure. Designed modifications to native primary and secondary structure have been incorporated to control the nanostructure and microstructure of the collagen-like materials produced. We find that the collagen-like molecules form a number of lyotropic rod liquid crystalline phases, which because of their strong temperature dependence in the liquid state can also be viewed as solvent intercalated thermotropic liquid crystals. The liquid crystalline phases formed by the molecules can be captured in the solid state by drying off solvent, resulting in solid nanopatterned (chemically and physically) thermally stable (to greater than 100 C) materials. Designed sequences which stabilize smectic phases have allowed a variety of nanoscale multilayered biopolymeric materials to be developed. Preliminary investigations suggest that chemical patterns running perpendicular to the smectic layer plane can be functionalized and used to localize a variety of organic, inorganic, and organometallic moieties in very simple multilayered nanocomposites. The phase behavior of collagen-like oligopeptide materials is described, emphasizing the correlation between mesophase, molecular orientation, and chemical patterning at the microscale and nanoscale. In many cases, the textures observed for smectic and hexatic phase collagens are remarkably similar to the complex (and not fully understood) helicoids observed in biological collagen-based tissues. Comparisons between biological morphologies and collagen model liquid crystalline (and solidified materials) textures may help us understand the molecular features which impart order and function to the extracellular matrix and to collagen-based mineralized tissues. Initial studies have utilized synthetic collagen-like peptides while future work will also focus on similar sequences generated via genetic engineering methods.

Valluzzi, Regina↗

Molecular chaperone properties of the high molecular weight aggregate from aged lens

The high molecular weight aggregate (HMWA) fraction was isolated from the water soluble proteins of aged bovine lenses. Its composition and ability to inhibit heat-induced denaturation and aggregation were compared with the lower molecular weight, oligomeric fraction of alpha isolated from the same lens. Although the major components of both fractions were the alpha-A and alpha-B chains, the HMWA fraction possessed a decreased ability to protect other proteins against heat-induced denaturation and aggregation. Immunoelectron microscopy of both fractions demonstrated that alpha particles from the HMWA fraction contained increased amounts of beta and gamma crystallins, bound to a central region of the supramolecular complex. Together, these results demonstrate that alpha crystallins found in the HMWA fraction possess a decreased ability to protect against heat-induced denaturation and aggregation, and suggest that at least part of this decrease could be due to the increased presence of beta and gamma crystallins complexed to the putative chaperone receptor site of the alpha particles.

NASA Discipline Developmental Biology↗

Crystallization Kinetics of a Solid Oxide Fuel Cell Seal Glass by Differential Thermal Analysis

Crystallization kinetics of a barium calcium aluminosilicate glass (BCAS), a sealant material for planar solid oxide fuel cells, have been investigated by differential thermal analysis (DTA). From variation of DTA peak maximum temperature with heating rate, the activation energy for glass crystallization was calculated to be 259 kJ/mol. Development of crystalline phases on thermal treatments of the glass at various temperatures has been followed by powder x-ray diffraction. Microstructure and chemical composition of the crystalline phases were investigated by scanning electron microscopy and energy dispersive spectroscopic (EDS) analysis. BaSiO3 and hexacelsian (BaAl2Si2O8) were the primary crystalline phases whereas monoclinic celsian (BaAl2Si2O8) and (Ba(x), Ca(y))SiO4 were also detected as minor phases. Needle-shaped BaSiO3 crystals are formed first, followed by the formation of other phases at longer times of heat treatments. The glass does not fully crystallize even after long term heat treatments at 750 to 900 C.

Bansal, Narottam P.↗

Titania Deposition on PMR-15

The formation, degree of crystallinity and adherence of dense titania (TiO2) thin film coatings on a high-temperature polyimide resin (PMR-15) can be influenced by the chemical composition of the polymer surface. Furthermore, solution deposition conditions can be adjusted to provide additional control over the morphology and crystallinity of the titania films. Recipes for solution-based titania deposition that used a slowly-hydrolyzing titanium fluoride salt in the presence of boric acid as a fluoride scavenger allowed growth of films up to 750 nm thick in 22 h. By adjusting solution pH and temperature, either amorphous titania or oriented crystalline anatase films could be formed. Surface sulfonate groups enhance the adhesion of solution-deposited oxide thin film coatings. While most sulfonation procedures severely damaged the PMR-15 surface, the use of chlorosulfonic acid followed by hydrolysis of the installed chlorosulfonyl groups provided effective surface sulfonation without significant surface damage. In some cases, the oxide deposition solution caused partial hydrolysis of the polymer surface, which itself was sufficient to allow adhesion of the titania film through chelation of titanium ions by exposed benzoic acid groups on the polymer surface.

Meador, Mary B.↗

Insights Developed Into the Damage Mechanism of Teflon FEP Thermal Control Material on the Hubble Space Telescope

Metalized Teflon FEP (DuPont; fluorinated ethylene propylene) thermal control material on the Hubble Space Telescope (HST) has been found to degrade in the space environment. Teflon FEP thermal control blankets retrieved during the first servicing mission were found to be embrittled on solar-facing surfaces and to contain microscopic cracks (the FEP surface is exposed to the space environment). During the second servicing mission, astronauts noticed that the FEP outer layer of the multilayer insulation blanketing covering the telescope was cracked in many locations. Large cracks were observed on the light shield, forward shell, and equipment bays. A tightly curled piece of cracked FEP from the light shield was retrieved during the second mission. This piece was severely embrittled, as witnessed by ground testing. A Failure Review Board was organized by NASA Goddard Space Flight Center to determine the mechanism causing the multilayer insulation degradation. This board included members of the Electro-Physics Branch of the NASA Glenn Research Center at Lewis Field. Density measurements of the retrieved materials obtained under the review board's investigations indicated that FEP from the first servicing mission was essentially unchanged from pristine FEP but that the second servicing mission FEP had increased in density in comparison to pristine FEP (ref. 1). The results were consistent with crystallinity measurements taken using x-ray diffraction and with results from solid-state nuclear magnetic resonance tests (see the table and ref. 1). Because the second servicing mission FEP was embrittled and its density and crystallinity had increased in comparison to pristine FEP, board researchers expected that the first servicing mission FEP, which was also embrittled, would also have increased in crystallinity and density, but it did not. Because the retrieved second servicing mission material curled while in space, it experienced a higher temperature extreme during thermal cycling (estimated at 200 C) than the first servicing mission material (estimated at 50 C). Therefore, Glenn initiated and conducted an investigation of the effects of heating pristine FEP and FEP that had been exposed on the Hubble Space Telescope. Samples of pristine and first and second servicing mission FEP were heated to 200 C and evaluated for changes in density and morphology. We hoped that the results would help explain why FEP degrades in the Hubble Space Telescope space environment.

deGroh, Kim K.↗