Development of protective finishes for glass monofilaments Final report
Organic and nickel metal protective finishes to prevent degradation of stength of glass filaments in resin-glass composites
PROTECTIVE COATING↗
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Effects of long term space environment exposure on optical substrates and coatings (S0050-2)
The experiment consisted of Fused Silica and Ultra Low Expansion (ULE(tm)) glass samples which were either uncoated or had high reflectance silver, antireflectance, or solar rejection coatings. A set of duplicate control samples was manufactured and stored in a controlled environment for comparison purposes. We will present spectral curves for the glass and coatings which define preflight, postflight, and post-cleaning performance. Data on the analysis of the contaminate deposited on the samples and stress measurements in the glass will also be presented. Some results of particular interest are that the contaminate composition varied between different types of samples, and no darkening of the ULE(tm) glass occurred due to the radiation exposure.
Vallimont, John↗
Multi-cell, triple pane, vacuum insulated glazing
A novel Triple Pane Vacuum Insulated Glazing (TPVIG) architecture consisting of three panes of glass separated by two offset grids is described. The grids are made of frit-coated fibers fused with the glass panes in a vacuum to create many independent hermetic cells. Unlike traditional VIGs, which are separated by support pillars, these cells significantly increase the redundancy in sealing, and the additional bonds formed by the grid lines reduce the stresses on the edge bonds thereby increasing VIG reliability. A numerical thermal analysis was conducted to determine the thermal performance of the VIG and suggested U-values below 0.5 W/m 2 -K (greater than R=11.4 hr-ft 2 -°F/Btu) can be obtained. A prototype of the VIG unit consisting of three glass panes (5.7 mm, 1.1 mm and 5.7 mm thick with low-e coating on two surfaces) was fabricated and tested for thermal performance using the hot box method. The experimental center of glass U-value for the VIG was found to be 0.42 W/m 2 K (R=13.2 hr-ft 2 -°F/Btu). Furthermore, this U-value is about four times lower than a typical Argon filled double pane window.
14 SOLAR ENERGY↗
Advanced Al Mirrors Protected with LiF Overcoat to Realize Stable Mirror Coatings for Astronomical Telescopes
Pure Aluminum (Al) exhibits intrinsic high reflectance over the proposed Large UV/Optical/IR (LUVOIR) Surveyor observatory target spectral range (90-2500 nm). However, Al coatings have to be protected from oxygen exposure in order to prevent the formation of the naturally occurring Al2O3 oxide layer, which limit performance for use only above 160 nm. Aluminum protected with fluorides such as LiF or MgF2 have been the most commonly used solutions. But below 102 nm and down to 90 nm, no transparent material is available to protect Al and coating mirror reflectance stays below 40%. But even above 102 nm, the reflectance of protected Al is limited by the residual absorption of the fluoride overcoats. Hence, this paper will report on recent advances in producing enhanced Al-based mirror coatings with the highest possible far-ultraviolet (FUV) reflectance, while exhibiting a more stable LiF protection layer. The process starts with a bare optically smooth glass substrate that is coated with Al in an ultra-high vacuum chamber by using the physical vapor deposition (PVD) process, which has been shown to provide the best aluminum thin-films when compared to other approaches. The next step is done by in-situ exposure of the freshly made Al film to a reactive XeF2 gas that will grant a thin AlF3 overcoat (2-3 nm) to the Al film that prevents further oxidation. This fluorinated Al film is then coated with a final layer of a LiF metal-fluoride overcoat. The coating process is finalized with a second exposure to the XeF2 precursor gas. The preparation of these mirror coatings will be studied and analyzed as a function of the XeF2 exposure time and deposition rate of the LiF layer during the PVD process. This paper will present and discuss characterization of a number of Al+XeLiF witness coupons produced with this reactive PVD (rPVD) process. These studies include characterization of specular reflectance in the 90-2500 nm spectral range, micro-roughness, long-term stability, as well as polarization characteristics in the visible and near-infrared spectral regions. These studies have been performed in order to demonstrate the improved reflectance performance, longer durability, and less hygroscopic nature of protected Al mirrors produced with the rPVD process (through exposure to XeF2) and in comparison with the standard PVD process.
optics↗
Thermal Stress Analysis of RCG-Tempered TUFI Tile TPS for Hypersonic Vehicles
This paper presents detailed results from linear and nonlinear finite-element thermal stress analyses of a new tile, Thermal Protection Systems (TPS) concept. A very thin coating of Reaction Cured Glass (RCG) is used to "temper" the surface of Toughened Uni-Piece Fibrous Insulation (TUFI) tiles to improve resistance to thermal shock and thermal cycling effects. The coating also serves to reduce catalytic heating and may improve waterproofing. Calculations include trajectory-based aerothermal heating environments for X-34 wing leading edge TPS designs and arc jet environments for TPS test articles. The nonlinear analyses include the high temperature plasticity of RCG to demonstrate the reuseability of the material.
Milos, Frank S.↗
New Fiber Reinforced Waterless Concrete for Extraterrestrial Structural Applications
Commercial use of sulfur concrete on Earth is well established, particularly in corrosive, e.g., acid and salt, environments. Having found troilite (FeS) on the Moon raises the question of using extracted sulfur as a lunar construction mate: iii an attractive alternative to conventional concrete as it does not require water For the purpose of this paper it is assumed that lunar ore is mined, refined, and the raw sulfur processed with appropriate lunar regolith to form, for example, brick and beam elements. Glass fibers produced from regolith were used as a reinforcement to improve the mechanical properties of the sulfur concrete. Glass fibers and glass rebar were produced by melting the lunar regolith simulant. Lunar regolith stimulant was melted in a 25 cc Pt-Rh crucible in a Sybron Thermoline 46100 high temperature MoSi2 furnace at melting temperatures of 1450 to 1600G. The glass melt wets the ceramic rod and long continuous glass fibers were easily hand drawn. The glass fibers were immediately coated with a protective polymer to maintain the mechanical strength. The viability of sulfur concrete as a construction material for extraterrestrial application is presented. The mechanical properties of the glass fiber reinforced sulfur concrete were investigated.
Toutanji, H.↗
Polyimides Containing Amide And Perfluoroisopropyl Links
New polyimides synthesized from reactions of aromatic hexafluoroisopropyl dianhydrides with asymmetric amide diamines. Soluble to extent of at least 10 percent by weight at temperature of about 25 degrees C in common amide solvents such as N-methylpyrrolidone, N,N-dimethylacetamide, and N,N-dimethylformamide. Polyimides form tough, flexible films, coatings, and moldings. Glass-transition temperatures ranged from 300 to 365 degrees C, and crystalline melting temperatures observed between 543 and 603 degrees C. Display excellent physical, chemical, and electrical properties. Useful as adhesives, laminating resins, fibers, coatings for electrical and decorative purposes, films, wire enamels, and molding compounds.
Dezem, James F.↗
Apollo 17 ropy glasses
Ropy glasses are a major soil component in the Apollo 17 gray soils 74240 and 74260. These particles form a distinct morphological type characterized by a wide range of dynamic shapes with a diagnostic sorted and welded fine-grained debris coating. Apollo 17 ropy glasses show abundant evidence for shock. Shocked lithic and mineral inclusions, lack of any igneous textures, and lechatelierite, all indicate an impact origin. A striking similarity is observed between the lunar ropy glasses and the glass impact bombs (Flaedle) of the Ries Crater in Germany. A highland basaltic composition was observed for the Apollo 17 ropy glasses in contrast to the KREEP composition of ropy glasses from the Apollo 12 and Apollo 14 landing sites. Other workers have presented convincing evidence that ejecta from Tycho reached the Taurus-Littrow Valley, and these ropy glasses may represent Tycho ejecta. However, the close stratigraphic association of the ropy glasses with the greater than 3.5 b.y. old orange glass suggests the ropy glasses may be too old to be Tycho ejecta, which should be only about 100 m.y. old. If this is the case, the ropy glasses represent impact glasses from a very old impact in an unknown highlands source area.
Fruland, R. M.↗
Comparison under a simulated sun of two black-nickel-coated flat-plate solar collectors with a nonselective black-paint-coated collector
A performance evaluation was made of two, black nickel coated, flat plate solar collectors. Collector performance was determined under a simulated sun for a wide range of inlet temperatures, including the temperature required for solar powered absorption air conditioning. For a basis of comparison a performance test was made on a traditional, two glass, nonselective, black paint coated, flat plate collector. Performance curves and performance parameters are presented to point out the importance of the design variables which determine an efficient collector. A black nickel coated collector was found to be a good performer at the conditions expected for solar powered absorption air conditioning. This collector attained a thermal efficiency of 50 percent at an inlet temperature of 366 K (200 F) and an incident flux of 946 watts/sq m (300 Btu/hr-sq ft).
Simon, F. F.↗
The source of sublimates on the Apollo 15 green and Apollo 17 orange glass samples
Elemental analyses of the thin film of micromounds which coat the surfaces of Apollo 15 green glass and Apollo 17 orange glass are reported. It is thought that Zn, Ga, Pb, Cu, Tl, S, F, and Cl condensed as a sublimate on the outside surface of these glass particles in lava fountains about 3.4 and 3.6 b.y. ago (Apollos 15 and 17, respectively). The heavy metals enriched in these samples may have been mobilized in a halide- and sulfide-rich vapor, while the source of these elements and of the glass may be a sulfide- and halide-rich pyroxenite inside the moon. The isotopic composition of lead on the surface of individual particles was determined, and the composition is considered with respect to the evolution of the source region. The lead on the surfaces is similar to lead that has been mixed into other soils and breccias at nearby sites.
Meyer, C., Jr.↗
Repairing cracked glass
Filing procedure consisting of machined lightweight fused-silica tiles coated with thin-layer of borosilicate glass produces homogeneous seal in thin glass. Procedure is useful in repairing glass envelopes, X-ray tub windows, Dewar flasks, and similar thin glass objects.
Helman, D. D.↗
Effect of surface topography on structural growth of thick sputtered films
Primarily thick sputtered S-Monel, silver, and 304 stainless steel coatings were deposited on mica, glass, and metal substrates with various surface finishes to investigate the structural growth of the coating by scanning electron microscopy. Compositional changes within the coating were analyzed by X-ray dispersion microscopy. Defects in the surface finish act as preferential nucleation sites and form isolated and complex nodules and various surface overgrowths in the coating. These nodules do not disappear after full annealing. Further, they have undesirable effects on mechanial properties; cracks are initiated at the nodules when the coating is stressed by mechanical forces. These effects are illustrated by micrographs. Nodular growth within a coating can be minimized or eliminated by reducing the surface roughness.
Spalvins, T.↗
Polymer Coatings Reduce Electro-osmosis
Poly(ethylene glycol) film controls electrostatic potential. Electro-osmosis in quartz or glass chambers reduced or reversed by coating inside surface of chambers with monomacromolecular layers of poly(ethylene glycol). Stable over long times. Electrostatic potential across surface of untreated glass or plastic chamber used in electro-phoresis is negative and attracts cations in aqueous electrolyte. Cations solvated, entrains flow of electrolyte migrating toward cathode. Electro-osmotic flow interferes with desired electrophoresis of particles suspended in electrolyte. Polymer coats nontoxic, transparent, and neutral, advantageous for use in electrophoresis.
Herren, Blair J.↗
Exposure of Highly Reflective Far-Ultraviolet Coatings to LEO Environment for TRL Advancement for the Habitable Worlds Observatory
Over the past several years, our team at the NASA Goddard Space Flight Center (GSFC), in collaboration with the Jet Propulsion Laboratory (JPL) and the Naval Research Laboratory (NRL), have developed several new protected Al coating technologies with improved Far-Ultraviolet (FUV) reflectance performance and more robust environmental stability. These include Al protected with lithium-based fluoride (LiF) coatings such as hot deposited LiF (eLiF), XeF 2 -passivated LiF coatings (XeLiF), Li 3 AlF 6 overcoats, AlF 3 (plasma passivated), and XeF 2 passivated MgF 2 coatings (XeMgF 2 ). However, despite these developments, relatively little experimental information exists regarding the long-term stability of these coatings after simultaneous exposure to the Low Earth Orbit (LEO) environment. To evaluate their environmental durability and advance their Technology Readiness Level (TRL), representative samples of these coating technologies, Al+XeLiF, Al+eLiF, Al+Li 3 AlF 6 , Al+AlF 3 , Al+XeMgF 2 , and bare Al as reference samples, were flown onboard the International Space Station (ISS) as part of the Materials International Space Station Experiment 20 (MISSE-20). The MISSE platform is operated by Aegis Aerospace for relatively long-duration (e.g. 6 months) external exposure experiments in a space environment. The coatings were deposited on ULE and Zerodur substrates, and witness samples deposited on the same coatings runs, but on glass slides were left on Earth as control. A subset of the flight samples were fitted with MgF 2 windows to reduce direct exposure to atomic oxygen (AO) and charged particles, and still let through UV and other types of radiation on these samples. After approximately 6 months of exposure in the forward-facing (RAM) direction, the samples were returned to Earth and characterized by performing FUV/NUV/VIS/NIR reflectance measurements to quantify degradation, spectroscopic ellipsometry to evaluate coating thickness and optical constants, atomic force microscopy (AFM) to quantify surface roughness evolution during the flight in the ISS. The MgF 2 protective windows were also analyzed through FUV transmission measurements. Comparison with the witness samples left on the ground and with the flown bare Al samples (with just the naturally occurring Al 2 O 3 layer) provided a quantitative assessment of coating thickness variations, optical performance degradation, and morphological changes induced by prolonged exposure to the LEO environment.
Far Ultraviolet (FUV)↗
Electrochemical Modeling of PID Leakage Current of PV Modules: Steady-State Current, Transient Current, and RC-Equivalent Circuit
Potential-induced degradation (PID) remains a significant reliability concern for photovoltaic (PV) modules, arising when a voltage difference between the module frame and the solar cells drives unintended leakage current through the glass-encapsulant stack. Although PID ultimately manifests as PID-s, PID-p, or PID-c, the underlying behavior of the leakage current-its magnitude and time dependence-requires clearer electrochemical interpretation. Traditional explanations attribute the initial transient current to bulk capacitive elements of the glass, encapsulant, and antireflection coatings, and the steady-state current according to their effective ohmic resistance. More recent studies, however, indicate that electrochemical charge-transfer processes at the encapsulant-metallization interface can play a dominant role in defining the leakage-current path. This paper develops a unified electrochemical framework for modeling PID leakage current. First, an RC-equivalent circuit is formulated by combining conventional RC elements with a Randles-type interface to capture transient leakage current through double-layer capacitance and faradaic processes at ionic-electronic boundaries. Second, the steady-state current-voltage behavior is explained using a linearized Butler-Volmer relationship, showing that the measured ohmic response corresponds to the low-overpotential limit of charge-transfer kinetics. Analytical results demonstrate that, for typical module materials-3.2-mm soda-lime glass and 0.45-mm encapsulant-the dominant modulators to PID leakage current are the glass surface resistance (under dry-surface conditions), the glass bulk capacitance, and the encapsulant resistance (under wet-surface conditions), with soda lime glass surface and EVA/POE encapsulant resistances primarily governing steady-state current. The proposed electrochemical model is validated against measured leakage-current data, showing good agreement in both the magnitude and the time-dependent evolution of PID leakage current.
14 SOLAR ENERGY↗
Improved Polyimide Intumescent Coating
New polyimide intumescent coating uses titanium dioxide and glass microballons as nucleating agents to improve foaming characteristics of commercially-available polyimide precursor resin. Used for coating interior surfaces in commercial aircraft.
Salyer, I. O.↗
TPS Materials and Costs for Future Reusable Launch Vehicles
There is considerable interest in developing new reusable launch vehicles (RLVs) for reducing the cost of transporting payload to and from orbit. This work reviews thirteen candidate thermal protection system (TPS) options currently available for RLVs. It is useful to begin with the current Shuttle TPS layout as a reference. The nose cap and wing leading edge , which reach the highest temperatures, are made of reinforced carbon-carbon (RCC) that is protected from oxidation by an external coating (about 0.020" thick) of silicon-carbide. Most of the windward surface is 9 lb/cubic ft ceramic tiles (LI-900) with a thin (about 0.012") coating of Reaction Cured Glass (RCG). The leeward side of the vehicle is covered largely by AFRSI, a quilted ceramic blanket, and FRSI, a polyamide felt. These four materials can be considered first generation reusable TPS. Since the time of the Shuttle design, considerable progress has been made advancing TPS technologies in terms of thermal performance, robustness, and cost. For each of the major systems, a second generation ceramic TPS has been developed, tested, and characterized. Metallic-based systems have also been developed. For applications requiring RCC in the past, advanced carbon-carbon (ACC) is now available. This material has better mechanical properties, somewhat higher temperature capability to 2900F and greatly increased oxidation resistance. New carbon fiber reinforced silicon-carbide matrix composites (C/SiCs) have shown additional improvement in properties over ACC with use temperatures to 3000F and above. For rigid tiles, NASA Ames has made two significant advancements. The first is a tile substrate called Alumina Enhanced Thermal Barrier, or AETB, that incorporates alumina fibers for improved dimensional stability at high temperatures, to 2600F and above. This material can be made to densities as low as 8 lb/cubic ft. The second is a coating preparation called Toughened Uni-piece Fibrous Insulation, or TUFT, that penetrates about 0.1 in. into the tile substrate. The resulting composite, with a functionally gradient density near the surface, provides orders of magnitude increased damage resistance compared with RCG coated LI-900, with only a small weight increase. The TPS that combines these two developments is called AETB-8/TUFI and has been adopted for high damage areas on the Shuttles. Two notable developments have occur-red in flexible ceramic blanket technology. The first is aluminoborosilicate-based fibers with use temperatures of 2200F and above," in comparison to quartz and silica fiber used in AFRSI which have multi-use temperature limits of 1200 to 1400F. Blankets incorporating these new high temperature fibers are referred to as AFRSI-HT. The second is an integral weaving techniques that produces a fluted core blanket with a smoother surface and greater resistance to aero-acoustic noise, to levels as high as 170 dB. This Ames innovation is called Tailorable Advanced Blanket Insulation, or TABI. Finally, for felt-based TPS, Boeing is developing Polybenzimidazole Blanket Insulation, or PBI, with a multi-use temperature limit of 1000F and above, in contrast to Shuttle FRSI which has a multi-use temperature limit of about 700F. 1.6 NASA Langley and BF Goodrich (formerly Rohr Corp.) have led the development of metallic-based TPS. This activity uses essentially three approaches: metallic tiles which encase a fibrous ceramic batting in a box fabricated largely from metallic honeycombs, typically Nickel based alloys; metallic honeycomb sheets, made of Nickel-based alloys, incorporating a fibrous back-side insulation encapsulated in a metallic foil bag, providing reduced weight; and metallic multi-wall, which is comprised of dimpled Titanium metal sheets, which are stacked and then diffusion bonded at contact points to form the TPS. The Nickel-based systems can be used up to temperatures of about 1800F, and the Titanium system to about 100F. These thirteen TPS materials have pros and cons to their usage in terms of temperature capability, weight, initial cost, and maintenance. Carbon-carbon and C/SiC systems have the highest temperature capability but are relatively expensive and heavy, requiring significant time, expertise, and costly facilities and tools for design and fabrication. Second generation ceramic tiles are relatively light, durable, simple to fabricate and easy to install; however, waterproofing is a concern. Blankets and felts are light, simple, inexpensive, and easy to install over curved vehicle surfaces, but durability and waterproofing are concerns. Metallics are robust and appear to have eliminated waterproofing, but they tend to be heavy and relatively expensive, requiring costly facilities and tools. If thin metal sheets are used to reduce weights, then issues arise from possible metal fatigue and corrosion caused by thermal cycling, pressure oscillations, and environmental exposure. For application to future RLVs, system analyses show that a significant component of the vehicle life cycle cost is from the TPS; however, it is difficult to quantify and to compare the potential savings of advanced systems without performing full vehicle designs using each of the different options. Because this entails a considerable effort and also tends to submerge TPS cost impacts under unrelated vehicle design assumptions, there is a clear need for a simpler quantitative method to evaluate the cost impact of different TPS options. To this end, this work introduces a TPS life-cycle cost parameter which is easily computed and applicable to generic RLVs.
Rasky, Dan J.↗
Bona fide upcycling strategy of anhydride cured epoxy and reutilization of decomposed dual monomers into multipurpose applications
Waste epoxy materials become an enormous problem to society and the environment. The advantages of epoxy resins derive from their rigid and chemically stable networks, but these qualities also make them difficult to dispose of or recycle. In this work, we demonstrated an efficient degradation of anhydride cured epoxy resin by aminolysis in aminoethanol without using any catalysts. The epoxy resin was fully decomposed at 160 °C in 4 h, resulting in two distinct high purity monomers (HHPA-OH and BPA-OH). To fully realize this upcycling approach, The BPA-OH was used to synthesize a polyurethane coating with an excellent glass transition temperature (88.9 °C), scratch hardness (8H), gouge hardness (6H), adhesive strength (5B), and strong solvent resistance. The HHPA-OH with two hydroxyl groups was reacted with methacrylic anhydride to form a dimethacrylate monomer which was then used as a viable crosslinker for photo-curable 3D printing thermosetting polymer with tensile strength as high as 64 MPa and impact strength of 4.86 kJ/m 2 . This work demonstrates a feasible pathway to convert anhydride cured epoxy waste to new monomeric recyclates for superior polymer products.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗