ALBERT

Description: Luminescent molecular probes imbedded in a polymer binder form a temperature or pressure paint. On excitation by light of the proper wavelength, the luminescence,which is quenched either thermally or by oxygen, is detected by a camera or photodetector. From the detected luminescent intensity, temperature and pressure can be determined. Tl e basic photophysics, calibration, accuracy and the response of a luminescent paints is described followed by applications in wind tunnels and in rotating machinery.

Description: Pressure-sensitive paint (PSP) and video model deformation (VMD) systems have been installed in the Unitary Plan Wind Tunnel at the NASA Langley Research Center to support the supersonic wind tunnel testing requirements of the High Speed Research (HSR) program. The PSP and VMD systems have been operational since early 1996 and provide the capabilities of measuring global surface static pressures and wing local twist angles and deflections (bending). These techniques have been successfully applied to several HSR wind tunnel models for wide ranges of the Mach number, Reynolds number, and angle of attack. A review of the UPWT PSP and VMD systems is provided, and representative results obtained on selected HSR models are shown. A promising technique to streamline the wind tunnel testing process, Modern Experimental Design, is also discussed in conjunction with recently-completed wing deformation measurements at UPWT.

Description: Pressure-sensitive paint (PSP) and video model deformation (VMD) systems have been installed in the Unitary Plan Wind Tunnel at the NASA Langley Research Center to support the supersonic wind tunnel testing requirements of the High Speed Research (HSR) program. The PSP and VMD systems have been operational since early 1996 and provide the capabilities of measuring global surface static pressures and wing local twist angles and deflections (bending). These techniques have been successfully applied to several HSR wind tunnel models for wide ranges of the Mach number, Reynolds number, and angle of attack. A review of the UPWT PSP and VMD systems is provided, and representative results obtained on selected HSR models are shown. A promising technique to streamline the wind tunnel testing process, Modern Experimental Design, is also discussed in conjunction with recently-completed wing deformation measurements at UPWT.

Description: The oxidative degradation of PMR (for polymerization of monomeric reactants) polyimides at elevated temperatures was followed by cross-polarized magic angle spinning (CP-MAS) NMR. Labeling of selected sites in the polymers with C-13 allowed for direct observation of the transformations arising from oxidation processes. The formation of several degradation products has been proposed to be occurring in the cross-links derived from the nadic end caps on oxidation. Model compounds have been synthesized and characterized by CPMAS NMR with both normal and delayed decoupling to distinguish between protonated and unprotonated carbons. Comparison of these spectra to predicted chemical shifts of proposed products for the aged polymer provides further insight to degradation occurring in the cross-linked moieties.

Description: A laser sintering/creep technique has been established to determine the creep behavior of thermal barrier coatings under steady-state high heat flux conditions. For a plasma sprayed zirconia-8 wt. % yttria coating, a significant primary creep strain and a low apparent creep activation energy were observed. Possible creep mechanisms involved include stress induced mechanical sliding and temperature and stress enhanced cation diffusion through the splat and grain boundaries. The elastic modulus evolution, stress response, and total accumulated creep strain variation across the ceramic coating are simulated using a finite difference approach. The modeled creep response is consistent with experimental observations.

Description: Efficient actuators that are lightweight, high performance and compact are needed to support telerobotic requirements for future NASA missions. In this work, we present a new class of electromechanically active polymers that can potentially be used as actuators to meet many NASA needs. The materials are graft elastomers that offer high strain under an applied electric field. Due to its higher mechanical modulus, this elastomer also has a higher strain energy density as compared to previously reported electrostrictive polyurethane elastomers. The dielectric, mechanical and electromechanical properties of this new electrostrictive elastomer have been studied as a function of temperature and frequency. Combined with structural analysis using x-ray diffraction and differential scanning calorimetry on the new elastomer, structure-property interrelationship and mechanisms of the electric field induced strain in the graft elastomer have also been investigated. This electroactive polymer (EAP) has demonstrated high actuation strain and high mechanical energy density. The combination of these properties with its tailorable molecular composition and excellent processability makes it attractive for a variety of actuation tasks. The experimental results and applications will be presented.

Description: The purpose of this paper is to evaluate the statistical molecular contamination data with a goal to improve spacecraft contamination control. The statistical data was generated in typical thermal vacuum tests at the National Aeronautics and Space Administration, Goddard Space Flight Center (GSFC). The magnitude of material outgassing was measured using a Quartz Crystal Microbalance (QCNO device during the test. A solvent rinse sample was taken at the conclusion of each test. Then detailed qualitative and quantitative measurements were obtained through chemical analyses. All data used in this study encompassed numerous spacecraft tests in recent years.

Description: During the Hubble Space Telescope (HST) Second Servicing Mission (SM2), degradation of unsupported Teflon(trademark) FEP (fluorinated ethylene propylene), used as the outer layer of the multi-layer insulation (MLI) blankets, was evident as large cracks on the telescope light shield. A sample of the degraded outer layer was retrieved during the mission and returned to Earth for ground testing and evaluation. The results of the Teflon(trademark) FEP sample evaluation and additional testing of pristine Teflon FEP led the investigative team to theorize that the HST damage was caused by thermal cycling with deep-layer damage from electron and proton radiation which allowed the propagation of cracks along stress concentrations, and that the damage increased with the combined total dose of electrons, protons, UV and x-rays along with thermal cycling. This paper discusses the testing and evaluation of the Teflon(trademark) FEP.

Description: In December 1993, the Environmental Protection Agency (EPA) Emission Standards Division and the National Aeronautics and Space Administration's (NASA's) Marshall Space Flight Center (MSFC) signed an Interagency Agreement (IA) initiating a task force for the technical assessment of alternative technologies for aerospace depainting operations. The United States Air Force (USAF) joined the task force in 1994. The mandates of the task force were: (1) To identify available alternative depainting systems that do not rely on methylene chloride or other ozone-depleting, chlorinated, and volatile organic carbon solvents. (2) To determine the viability, applicability, and pollution prevention potential of each identified alternative. (3) To address issues of safety, environmental impact, reliability, and maintainability. Through a Technical Implementation Committee (TIC), the task force selected and evaluated eight alternative paint stripping technologies: chemical stripping, carbon dioxide (CO2) blasting, xenon flashlamp and CO2 coatings removal (FLASHJET(R)), CO2 laser stripping, plastic media blasting (PMB), sodium bicarbonate wet stripping, high-pressure water blasting (WaterJet), and wheat starch abrasive blasting (Enviro-Strip(R)). (The CO2 blasting study was discontinued after the first depainting sequence.) This final report presents the results of the Joint EPA/NASA/USAF Interagency Depainting Study. Significant topics include: (1) Final depainting sequence data for the chemical stripping, PMB, sodium bicarbonate wet stripping, and WaterJet processes. (2) Strip rates for all eight technologies. (3) Sequential comparisons of surface roughness measurements for the seven viable depainting technologies. (4) Chronological reviews of and lessons learned in the conduct of all eight technologies. (5) An analysis of the surface roughness trends for each of the seven technologies. (6) Metallurgic evaluations of panels Summaries of corrosion and hydrogen embrittlement evaluations of chemical stripping panels, detailed descriptions of which appear in previous reports. Because the requirements for alternative systems are diverse, as are initial setup, training, and on-going operational considerations, this study does not recommend a particular product or process. Users of this study will draw their own conclusions from the data presented herein.

Description: The computational method described in this paper allows the calculation of the dielectric relaxation strength of an amorphous polymer based solely upon its chemical structure. The 4,4' oxydiphthalic anhydride (ODPA) dianhydride and bis-aminophenoxybenzene (APB) diamine based polyimides, (beta-CN) APB-ODPA and APB-ODPA were studied. Amorphous cells were constructed and then poled using molecular dynamics. Dielectric relaxation strengths of Delta(epsilon) = 17.8 for (beta-CN) APB-ODPA and Delta(epsilon) = 7.7 for APB-ODPA were predicted. These values are in excellent agreement with the experimental values. It was found that both the pendant nitrile dipole and the backbone anhydride residue dipole make significant contributions to the polyimides dielectric response. Specifically, it was shown that the difference in the magnitude of the dielectric relaxations is directly attributable to the nitrile dipole. The size of the relaxations indicate an absence of cooperative dipolar motions, The model was used to explain these results in terms of the average orientation of the nitrile and anhydride dipoles to within 51 deg. and 63 deg., respectively, of the applied electric field.

Description: During the Second Servicing Mission (SM2) of the Hubble Space Telescope (HST) severe degradation was observed on the outer layer of the thermal control blankets. Astronaut observations and photographs revealed large cracks in the metallized Teflon(trademark) FEP (fluorinated ethylene propylene), the outer layer of the multi-layer insulation (MLI), in many locations around the telescope. In an effort to understand what elements of the space environment might cause such damage, pristine Teflon(trademark) FEP was tested for durability to radiation and thermal cycling. Specimens were subjected to electron and proton fluences comparable to those experienced by HST and were subsequently thermal cycled in a custom-built rapid thermal cycle chamber. Tensile tests of the specimens showed that radiation followed by thermal cycling significantly reduced the ultimate strength and elongation of Teflon(trademark) FEP.

Description: This paper details a comparison analysis of the zinc-oxide pigmented white thermal control paints Z-93 and Z-93P. Both paints were simultaneously exposed to combined space environmental effects and analyzed using an in-vacuo reflectance technique. The dose applied to the paints was approximately equivalent to 5 yr in a geosynchronous orbit. This comparison analysis showed that Z-93P is an acceptable substitute for Z-93. Irradiated samples of Z-93 and Z-93P were subjected to additional exposures of ultraviolet (UV) radiation and analyzed using the in-vacuo reflectance technique to investigate UV activated reflectance recovery. Both samples showed minimal UV activated reflectance recovery after an additional 190 equivalent Sun hour (ESH) exposure. Reflectance response utilizing nitrogen as a repressurizing gas instead of air was also investigated. This investigation found the rates of reflectance recovery when repressurized with nitrogen are slower than when repressurized with air.

Description: The primary objective of this program is to produce deeply undercooled metallic liquids and to identify factors that limit undercooling and glass formation. The main research objectives are: (1) Investigating undercooling limits in glass-forming alloys and identifying factors that affect undercooling; (2) Measuring thermophysical properties and investigating the validity of the classical nucleation theory and other existing theories in the extreme undercooled states; and (3) To investigate the limits of electrostatic levitation technology in the ground base and to identify thermophysical parameters that might require reduced-g environment.

Description: Multi-body launch vehicles require the use of Solid Film Lubricants (SFLs) to allow for unrestricted relative motion between structural assemblies and components during lift-off and ascent into orbit. The Space Shuttle Solid Rocket Booster (SRB), uses a dual coat, ceramic-bonded high temperature SFL in several locations such as restraint hardware between the SRB aft skirt and the Mobile Launch Platform (MLP), the aft SRB/External Tank (ET) attach struts, and the forward skirt SRB/ET attach ball assembly. Future launch systems may require similar applications of SFLs for attachment and restraint hardware. A family of environmentally compatible non-lead/antimony bearing alternative SFLs have been developed including a compatible repair material. In addition, commercial applications for SFLs on transportation equipment, all types of lubricated fasteners, and energy related equipment allow for wide usage's of these new lubricants. The new SFLs trade named BOOSTERLUBE is a family of single layer thin film (0.001 inch maximum) coatings that are a unique mixture of non-hazardous pigments in a compatible resin system that allows for low temperature curing (450 F). Significant savings in energy and processing time as well as elimination of hazardous material usage and disposal would result from the non-toxic one-step SFL application. Compatible air-dry field repair lubricants will help eliminate disassembly of launch vehicle restraint hardware during critical time sensitive assembly operations.

Description: The objective of this new research project is to demonstrate by experiment, supplemented by mathematical modeling and physical property measurement, that the effects of buoyancy driven convection can be largely eliminated in ground-based experiments, and further reduced in flight, by applying a new technique. That technique exploits the dependence of magnetic susceptibility on composition or temperature. It is emphasized at the outset that the phenomenon to be exploited is fundamentally and practically different from the magnetic damping of convection in conducting liquids that has been the subject of much prior research. The concept suggesting this research is that all materials, even non-conductors, when placed in a magnetic field gradient, experience a force. Of particular interest here are paramagnetic and diamagnetic materials, classes which embrace the "model alloys", such as succinonitrile-acetone, that have been used by others investigating the fundamentals of solidification. Such alloys will exhibit a dependence of susceptibility on composition. The consequence is that, with a properly oriented field (gradient) a force will arise that can be made to be equal to, but opposite, the buoyancy force arising from concentration (or temperature) gradients. In this way convection can be stilled. The role of convection in determining the microstructure, and thereby properties, of materials is well known. Elimination of that convection has both scientific and technological consequences. Our knowledge of diffusive phenomena in solidification, phenomena normally hidden by the dominance of convection, is enhanced if we can study solidification of quiescent liquids. Furthermore, the microstructure, microchemistry and properties of materials (thereby practical value) are affected by the convection occurring during their solidification. Hitherto the method of choice for elimination of convection has been experimentation in microgravity. However, even in low Earth orbit, residual convection has effects. That residual convection arises from acceleration (drag on the spacecraft), displacement from the center of mass or transients in the gravitational field (g-jitter). There is therefore a need for both further reducing buoyancy driven flow in flight and allowing the simulation of microgravity during ground based experiments. Previous investigations, the research project description, theory behind the study and experimental methods as well as plots of magnetic fields and forces are presented.

Description: Resulting from a SBIR contract with the Goddard Space Flight Center, Foster-Miller developed a high performance, low cost substrate for printed circuits with a coefficient of thermal expansion (CTE) matched to the surface mounted devices. The commercial product that resulted from the agreement between the two organizations was so successful that Foster-Miller created a spin-off company named Superex, Inc., devoted solely to the promotion of this particular substrate. The contract originated from NASA's need to develop better, more cost effective satellite and land based electronic applications.

Description: Javelin, a Lone Peak Engineering Inc. Company has introduced the SteamRoller(TM) System as a commercial product. The system was designed by Javelin during a Phase II NASA funded small commercial product. The purpose of the invention was to allow automated-feed of flexible ceramic tapes to the Laminated Object Manufacturing rapid prototyping equipment. The ceramic material that Javelin was working with during the Phase II project is silicon nitride. This engineered ceramic material is of interest for space-based component.

Description: During the Hubble Space Telescope (HST) second servicing mission, astronauts noticed that the outer layer of the multilayer insulation (MLI) was cracked in many locations around the telescope. The insulation s outer layer is composed of 5-mil (0.127 mm) Teflon FEP (DuPont; fluorinated ethylene propylene) with vapor-deposited aluminum (VDA) on the backside. The MLI blankets, which are used on over 80 percent of the external surface of the telescope, provide passive thermal control for equipment. Two large cracks were observed on the light shield directly above the high gain antenna. The upper light shield crack propagated from a cut placed in the blanket during installation around a handrail standoff. Two cracks propagated almost normal to each other, with the outer layer curling tightly as the cracks propagated. A second much larger vertical crack had started to curl and lift away from the telescope, as seen in the figure. MLI on the equipment bays was cracked extensively also, and in some areas it had pulled away from the bay. Continued degradation of the equipment bay insulation would potentially cause limited observations because of housekeeping boxes; for example, the data interface unit could overheat during some portions of the year, in certain sun angles.

Description: During the Hubble Space Telescope (HST) Second Servicing Mission, 6.8 years after the telescope was deployed in low Earth orbit, degradation of unsupported Teflon FEP (DuPont; fluorinated ethylene propylene), used as the outer layer of the multilayer insulation (MLI) blankets, was evident as large cracks on the telescope light shield. A sample of the degraded outer layer (see the photograph) was retrieved during the second servicing mission and returned to Earth for ground testing and evaluation. Also retrieved was a Teflon FEP radiator surface from a cryogen vent cover that was exposed to the space environment on the aft bulkhead of the HST. NASA Goddard Space Flight Center directed the efforts of the Hubble Space Telescope MLI Failure Review Board, whose goals included determining the FEP degradation mechanisms. As part of the investigations into the degradation mechanisms, specimens retrieved from the first and second HST servicing missions, 3.6 and 6.8 years after launch, respectively, were characterized through exhaustive mechanical, optical, and chemical testing. Testing led by Goddard included scanning electron microscopy, optical microscopy, tensile testing, solar absorptance measurements, time-of-flight secondary ion mass spectroscopy (TOF-SIMS), Fourier transform infrared microscopy (m-FTIR), attenuated total reflectance infrared microscopy (ATR/FTIR), and x-ray diffraction (XRD). The NASA Lewis Research Center contributed significantly to the analysis of the retrieved HST materials by leading efforts and providing results of bend testing, surface microhardness measurements, x-ray photoelectron spectroscopy, solid-state nuclear magnetic resonance spectroscopy, and density measurements. Other testing was conducted by Nano Instruments, Inc., and the University of Akron.

Description: To meet the increased thermal stresses of future advanced aircraft engines, new lubricants will have to be developed to replace the currently used ester-based liquid lubricants. If a suitable conventional replacement cannot be found, a different lubrication method will have to be used. The conventional method circulates bulk lubricant (stored in a sump) through a lubricating system containing cooling and filtering elements. Solid lubricants have been studied as a replacement for bulk liquid lubricants, and have been found to provide reasonable lubrication for lightly loaded systems. Solid lubricants, however, have proved inadequate for highly loaded, high-speed applications. Vapor/mist phase lubrication (VMPL), on the other hand, may be a viable alternative. VMPL has been used successfully to lubricate high-temperature bearings or gears. It can be used as an emergency backup system or as the primary source of lubrication. With VMPL, minimal weight is added to the system and minimal debris is formed. It works over a wide temperature range.

Description: Small-diameter structural fibers are being considered as reinforcements for high temperature ceramic matrix composite materials, and thus they require characterization. At the NASA Lewis Research Center, a nondestructive optical technique was used to determine surface strain on a structural fiber, in real time, as it was pulled in a tensile test machine. With this technique, interference or speckle patterns from the laser illuminated fiber test specimen are recorded. As the fiber is pulled, its speckle pattern shifts in proportion to the strain, translation, and rotation components of the sample deformation. Shifting speckle patterns are detected in real time by two linear charge-coupled discharge (CCD) camera arrays, and the images are processed by a hardware correlator. Surface strain is selectively detected on fibers with diameters on the order of 100 mm and can be resolved to 19 microstrain. This system was designed to be robust and compact and generally does not require surface preparation of the structural fibers. For strain detection, two laser beams are positioned incident on the structural fiber being tested, as shown in the photograph, where the test specimen is mounted in a tensile test machine via two coupons. As the fiber is pulled, the speckle pattern produced from each laser beam is detected by one of two CCD arrays located inside the tube on the right side of the photograph.

Description: Ceramic matrix composites (CMC's) require strong fibers for good toughness and weak interphases so that cracks which are formed in the matrix debond and deflect around the fibers. If the fibers are strongly bonded to the matrix, CMC's behave like monolithic ceramics (e.g., a ceramic coffee cup), and when subjected to mechanical loads that induce cracking, such CMC's fail catastrophically. Since CMC's are being developed for high temperature corrosive environments such as the combustor liner for advanced High Speed Civil Transport aircraft, the interphases need to be able to withstand the environment when the matrix cracks.

Description: A piezoelectric polymeric blend system has been developed. The system contains two components: ferroelectric poly(vinylidene-trifluoroethylene) and graft elastomer. The remanent polarization, Pr, and the piezoelectric strain coefficient, d31, of the blends have been studied as a function of relative composition of the two components, temperature and frequency. Both blended copolymer and graft unit in the elastomer contribute to the total crystallinity of the blend-system, and hence to the remanent polarization and piezoelectricity. The piezoelectric strain coefficient, d31, of the blend systems shows dependence on both the remanent polarization and the mechanical stiffness, which in turn are determined by the fraction of the two components in the blends. This mechanism makes it possible for the piezoelectric strain response of the blend to be tailored by adjusting the relative composition. Although Pr of the copolymer is higher than that of the blends, the blend films containing 75 wt.% copolymer exhibit a higher d31 at room temperature, possibly due to their lower modulus. The blend films containing 50 wt.% copolymer exhibit a constant value of d31, from room temperature to 70 C.

Description: The accurate determination of inert strength is important in reliable life prediction of structural ceramic components. At ambient temperature, the inert strength of a brittle material is typically regarded as free of the effects of slow crack growth due to stress corrosion. Therefore, the inert strength can be determined either by eliminating active species, especially moisture, with an appropriate inert medium, or by using a very high test rate. However, at elevated temperatures, the concept or definition of the inert strength of brittle ceramic materials is not clear, since temperature itself is a degrading environment, resulting in strength degradation through slow crack growth and/or creep. Since the mechanism to control strength is rate-dependent viscous flow, the only conceivable way to determine the inert strength at elevated temperatures is to utilize a very fast test rate that either minimizes the time for or eliminates slow crack growth. Few experimental studies have measured the elevated-temperature, inert (or "ultra"-fast fracture) strength of advanced ceramics. At the NASA Lewis Research Center, an experimental study was initiated to better understand the "ultra"-fast fracture strength behavior of advanced ceramics at elevated temperatures. Fourteen advanced ceramics - one alumina, eleven silicon nitrides, and two silicon carbides - have been tested using constant stress-rate (dynamic fatigue) testing in flexure with a series of stress rates including the "ultra"-fast stress rate of 33 000 MPa/sec with digitally controlled test frames. The results for these 14 advanced ceramics indicate that, notwithstanding possible changes in flaw populations as well as flaw configurations because of elevated temperatures, the strength at 33 000 MPa/sec approached the room-temperature strength or reached a higher value than that determined at the conventional test rate of 30 MPa/sec. On the basis of the experimental data, it can be stated that the elevated-temperature, inert strength of an advanced ceramic material can be defined as the strength where no slow crack growth takes place at the temperature.

Description: Development of accurate three-dimensional (multiaxial) inelastic stress-strain models is critical in utilizing advanced ceramics for challenging 21st century high-temperature structural applications. The current state of the art uses elastic stress fields as a basis for both subcritical crack growth and creep life prediction efforts aimed at predicting the time dependent reliability response of ceramic components subjected to elevated service temperatures. However, to successfully design components that will meet tomorrow's challenging requirements, design engineers must recognize that elastic predictions are inaccurate for these materials when subjected to high-temperature service conditions such as those encountered in advanced heat engine components. Analytical life prediction methodologies developed for advanced ceramics and other brittle materials must employ accurate constitutive models that capture the inelastic response exhibited by these materials at elevated service temperatures. A constitutive model recently developed at the NASA Lewis Research Center helps address this issue by accounting for the time-dependent (inelastic) material deformation phenomena (e.g., creep, rate sensitivity, and stress relaxation) exhibited by monolithic ceramics exposed to high-temperature service conditions. In addition, the proposed formulation is based on a threshold function that is sensitive to hydrostatic stress and allows different behavior in tension and compression, reflecting experimental observations obtained for these material systems.

Description: The High Temperature Integrated Electronics and Sensors (HTIES) team at the NASA Lewis Research Center is developing silicon carbide (SiC) as an enabling electronic technology for many aerospace applications. The Lewis team is focusing on the chemical vapor deposition of the thin, single-crystal SiC films from which devices are fabricated. These films, which are deposited (i.e., epitaxially "grown") on commercial wafers, must consist of a single crystal with very few structural defects so that the derived devices perform satisfactorily and reliably. Working in collaboration (NASA grant) with Professor Pirouz of Case Western Reserve University, we developed a chemical-mechanical polishing (CMP) technique for removing the subsurface polishing damage prior to epitaxial growth of the single-crystal SiC films.

Description: Norbornenyl-end capped PMR polyimide resins are widely used as polymer matrix composite materials for aircraft engine applications, since they combine ease of processing with good oxidative stability up to 300 C. PMR resins are prepared by a two-step approach involving the initial formation of oligomeric pre-polymers capped at both ends by a latent reactive end cap. The end cap undergoes cross-linking during higher temperature processing, producing the desired low density, high specific strength materials, for PMR- 15. The end cap facilitates processing by controlling the molecular weight of the oligomer and allowing flow before it cross-links. However, after cross-linking, this very end cap accounts for much of the weight loss in the polymer on aging in air at elevated temperatures. Understanding this degradation provides clues for designing new end caps to slow down degradation, and prolong the lifetime of the material.

Description: 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.

Description: The potential of pressure-sensitive paint (PSP) to provide aerodynamic loads measurements has been a driving force behind the development of this measurement technique. To demonstrate the suitability of PSP for this purpose, it is necessary to show that PSP-derived pressures can be accurately integrated over the model surface. This cannot be done simply by demonstrating the accuracy of PSP as compared to pressure taps. PSP errors due to misregistration or temperature sensitivity may be high near model edges, where they will have a strong effect on moment measurements, but where pressure taps are rarely installed. A more suitable technique is to compare integrated PSP data over the entire model surface with balance and/or CFD results. This paper presents results from three experiments in which integrated PSP data is compared with balance and/or CFD data. This allows the usefulness of PSP for force and moment measurements, and by implication for loads measurements, to be assessed.

Description: We analyze the onset of "necking" and subsequent filament failure during the transient uniaxial elongation of viscoelastic fluid samples in extensional rheometers. In the limit of rapid elongation (such that no molecular relaxation occurs), the external work applied is all stored elastically and the Considere criterion originally developed in solid mechanics can be used to quantitatively predict the critical Hencky strain to failure. By comparing the predictions of the Doi-Edwards model for linear homopolymer melts with those of the "Pom-Pom" model for prototypical branched melts we show that the critical strain to failure in rapid elongation of a rubbery material is intimately linked to the molecular topology of the chain, especially the degree of chain branching. The onset of necking instability is monotonically shifted to larger Hencky strains as the number of branches is increased. Numerical computations at finite Deborah numbers also show that there is an optimal range of deformation rates over which homogeneous extensions can be maintained to large strain. We also consider other rapid homogeneous stretching deformations, such as biaxial and planar stretching, and show that the degree of stabilization afforded by inclusion of material with long-chain branching is a sensitive function of the imposed mode of deformation.

Description: The current Space Shuttle Reusable Solid Rocket Motor (RSRM) nozzle adhesive bond system is being replaced due to obsolescence. Down-selection and performance testing of the structural adhesives resulted in the selection of two candidate replacement adhesives, Resin Technology Group's Tiga 321 and 3M's EC2615XLW. This paper describes rocket motor testing of these two adhesives. Four forty-pound charge motors were fabricated in configurations that would allow side by side comparison testing of the candidate replacement adhesives and the current RSRM adhesives. The motors provided an environment where the thermal performance of adhesives in flame surface bondlines was compared. Results of the FPC testing show that: 1) The phenolic char depths on radial bond lines is approximately the same and vary depending on the position in the blast tube regardless of which adhesive was used; 2) The adhesive char depth of the candidate replacement adhesives is less than the char depth of the current adhesives; 3) The heat-affected depth of the candidate replacement adhesives is less than the heat-affected depth of the current adhesives; and 4) The ablation rates for both replacement adhesives are slower than that of the current adhesives.

Description: The use of polymer matrix composites (PMC's) in aircraft engines can lead to substantial weight savings over metals. This weight reduction correlates into better fuel economy, increased speed, and increased passenger load. Typically, high performance PMC's possess high thermal-oxidative stabilities (TOS) and high glass transition temperatures (Tg's) to withstand temperatures up to 316 C (600 F). One of the leading high temperature resins system available today is PMR-15 (Polymerization of Monomeric Reactants, MW=1500). This thermosetting polyimide utilizes addition curing through polymer endcaps which enables hand lay-up processing of carbon fiber composite parts with low void contents. However, the large amount of hand labor raises manufacturing costs and prohibits the use of PMR-15 in many aerospace applications. Resin Transfer Molding (RTM) provides an economical alternative, but it requires a melt Viscosity of less than 10(exp 3) centipoise (cP). This is much lower than the minimum melt viscosity of PMR-15 (about 10(exp 6) cP). To improve the processability of polyimides, the polymer backbone can be modified by incorporating flexible linkages, such as branching. bulky pendant groups, kinked structures, and twisted or non-coplanar moietes . The focus of this paper will be the introduction of non-coplanar biaryls into the PMR polyimide backbone to increase processability while maintaining high temperature performance.

Description: Plasma-sprayed mullite (3Al2O3 central dot 2SiO2) and mullite/yttria-stabilized-zirconia (YSZ) dual layer coatings have been developed to protect silicon-based ceramics from environmental attack. Mullite-based coating systems show excellent durability in air. However, in combustion environments, corrosive species such as molten salt or water vapor penetrate through cracks in the coating and attack the Si-based ceramics along the interface, Thus modification of the coating system for enhanced crack-resistance is necessary for long-term durability in combustion environments. Other key durability issues include interfacial contamination and coating/substrate bonding. Interfacial contamination leads to enhanced oxidation and interfacial pore formation, while weak coating/substrate bonding leads to rapid attack of the interface by corrosive species, both of which can cause premature failure of the coating. Interfacial contamination can be minimized by limiting impurities in coating and substrate materials. The interface may be modified to improve the coating/substrate bond.

Description: Pressure-sensitive paint (PSP) has become a useful tool to augment conventional pressure taps in measuring the surface pressure distribution of aerodynamic components in wind tunnel testing. While the PSP offers the advantage of a non-intrusive global mapping of the surface pressure, one prominent drawback to the accuracy of this technique is the inherent temperature sensitivity of the coating's luminescent intensity. A typical aerodynamic surface PSP test has relied on the coated surface to be both spatially and temporally isothermal, along with conventional instrumentation for an in situ calibration to generate the highest accuracy pressure mappings. In some tests however, spatial and temporal thermal gradients are generated by the nature of the test as in a blowing jet impinging on a surface. In these cases, the temperature variations on the painted surface must be accounted for in order to yield high accuracy and reliable data. A new temperature correction technique was developed at NASA Lewis to collapse a "family" of PSP calibration curves to a single intensity ratio versus pressure curve. This correction allows a streamlined procedure to be followed whether or not temperature information is used in the data reduction of the PSP. This paper explores the use of conventional instrumentation such as thermocouples and pressure taps along with temperature-sensitive paint (TSP) to correct for the thermal gradients that exist in aeropropulsion PSP tests. Temperature corrected PSP measurements for both a supersonic mixer ejector and jet cavity interaction tests are presented.

Description: Because of its high reactivity, atomic oxygen causes surface erosion on polymeric materials. although the reaction efficiency depends on the chemical structure of the polymer. We have found an organotin compound, bis(triphenyltin) oxide (BTO), which has an unusually high solubility in solutions of a number of commercial high performance polymers. Films of these polymers containing BTO showed a substantial reduction in erosion by atomic oxygen when compared with films of the pure material. Analysis has shown that in the presence of atomic oxygen, erosion of the exposed surfaces of the BTO-containing films leaves a residual protective tin oxide coating . Since the additive is uniformly distributed throughout the polymeric material, any break or puncture in the protective coating is "healed" by the material below. Samples were exposed to the environment of the low earth orbit (LEO) on two Space Shuttle flights, STS-46, in June of 1992, and STS-51 in September of 1993. The analysis of these samples has been reported previously. For both flights, the samples were small (1.3 cm and 1.9 cm respectively) thus limiting the scope of analysis. In the research under this cooperative agreement, films of a polyetherimide, were exposed to the LEO environment on Space Shuttle flight STS-85 in August of 1997 as part of the Evaluation of Space Environment and Effects on Materials (ESEM) experiment. The polyetherimide chosen is available commercially as Ultem, registered to the General Electric Company. Films of pure Ultem, Ultem with 10% BTO by mass, and Ultem with 20% BTO by mass were exposed in the ram direction for 40 hours during STS-85. Ultem has a Tg of 215 deg C and is soluble in common chlorinated solvents. Granules of the polymer were dried at 120 deg C, but otherwise were used as received. Films were cast on a glass plate from a solution of the polymer in a 60/40 (w/w) mixture of chloroform and 1,1,2,2-tetrachloroethane. The plate was placed in a dust-free box for at least 24 hours to allow much of the solvent to evaporate, and then was moved to a vacuum oven and slowly heated from 20 to 220 deg C over a period of two weeks to completely remove all solvent. Each exposed sample was 7.6 cm long and 2.2 cm wide and about 0.025 mm thick. The structures of Ultem and bis(triphenyltin) oxide are shown.

Description: Simulation of composites degradation due to aging are described. Laminate geometry, material properties, and matrix degradation states are specified as functions of position and time. Matrix shrinkage and property changes are modeled as functions of the degradation states. Aging effects at the laminate, ply, and micro levels are evaluated, to determine failure of any kind. The results obtained show substantial ply stress built up as a result of aging accompanied by comparable laminate strength degradation in matrix dominated composite strengths.

Description: The work presented in this paper was performed to identify and quantify the offgassing behavior of alternative re-waterproofmg materials under investigation for application to Shuttle Orbiter Thermal Protection System (TPS) tile and blanket materials. The purpose was to determine whether the new materials would cause a problem with the operational analysis of residual vapors using the current portable vapor analyzer, a Miran 203. The materials investigated were limited to dimethylethoxysilane (DMES) and proposed solvent selected as suitable for use in re-waterproofing Orbiter TPS. The solvent was selected in another phase of the overall project. Obiter TPS tiles were injected with the re-waterproofing materials under constant conditions of temperature, relative humidity and air flow. The vapor concentrations of offgassing materials were monitored using Fourier Transform Infrared (FTIR) multi-component analysis, and with the Miran 203 instruments. The procedure was to record the time dependent concentrations of offgassing materials as analyzed by the FTIR, and the time response of the Miran 203 to the materials under consideration. The FTIR was calibrated for vapor phase DMES, tetramethyldisiloxane (TMDS), ethanol and the hydrocarbon solvents to be used to dilute the DMES for application to the TPS tile. The Miran 203 was calibrated for the operational measurement of DMES airborne vapors. The FTIR data, shows for the first time that the principal product which offgases from the tile after the first hour is not DMES, but TMDS and ethanol. The Miran 203 response to TMDS is the primary reading after the re-waterproofing operation is completed. The operational use of the Miran 203 to measure DMES vapors after re-waterproofmg operations has been responding to TMDS. The results of this study suggest that the historical complaints that have contributed to the low threshold limit value (TLV) for DMES concentrations, as read with the Miran 203, are actually based on instrumental responses to TMDS, for which no other toxicology information is available at this time. While there is some interference, the use of the tested hydrocarbon solvents does not adversely affect the response of the Miran 203.

Description: A common component of multi-layer insulation blankets is beta cloth, a woven fiberglass cloth impregnated with Teflon. It is planned for extensive use on the International Space Station (ISS). The Environmental Effects Group of the Marshall Space Flight Center Materials, Processing and Manufacturing Department has investigated the impact of atomic oxygen (AO) and ultraviolet (UV) radiation on the optical properties of plain and aluminized beta cloth, both in the laboratory and as part of long-duration flight experiments. These investigations indicate that beta cloth was susceptible to darkening in the presence of UV radiation, dependent on the additives used. The presence of AO countered some, if not all, of the UV degradation.

Description: A low Earth orbital space experiment entitled, "Polymers Erosion And Contamination Experiment", (PEACE) has been designed as a Get-Away Special (GAS Can) experiment to be accommodated as a Shuttle in-bay environmental exposure experiment. The first objective is to measure the atomic oxygen erosion yields of approximately 40 different polymeric materials by mass loss and erosion measurements using atomic force microscopy. The second objective is to evaluate the capability of identifying sources of silicone contamination through the use of a pin-hole contamination camera which utilizes environmental atomic oxygen to produce a contaminant source image on an optical substrate.

Description: This report summarizes the last nine years research accomplishments under Cooperative Agreement NCC2-650 between NASA, Ames Research Center and SETI Institute. Four Major research tasks are conducted: 1. Gas chromatography column development. 2. Pyrosensor development. 3. Micro-machining gas chromatography instrument development. 4. Amino acid analysis and high molecular weight polyamino acid synthesis under prebiotic conditions. The following describes these results.

Description: An atmospheric atomic oxygen beam has been found to be effective in removing organic materials through oxidation that are typical of graffiti or other contaminant defacements which may occur to the surfaces of paintings. The technique, developed by the National Aeronautics and Space Administration, is portable and was successfully used at the Carnegie Museum of Art to remove a lipstick smudge from the surface of porous paint on the Andy Warhol painting "Bathtub." This process was also evaluated for suitability to remove felt tip and ball point ink graffiti from paper, gesso on canvas and cotton canvas.

Description: A series of displacement-controlled, conventional, drained axisymmetric (triaxial) experiments were conducted on dry Ottawa sand specimens at very low effective confining stresses in a microgravity environment aboard the Space Shuttle during the NASA STS-89 mission. Post-flight analysis included studying the internal fabric and failure patterns of these specimens using Computed Tomography (CT). The CT scans of three specimens subjected to different compression levels (uncompressed specimen, a specimen compressed to 3.3% nominal axial strain (epsilon(sub a)), and a specimen compressed to 25% epsilon(sub a)) are presented to investigate the evolution of instability patterns and to quantify void ratio variation. The progress of failure is described and discussed. Also, specimens' densities were calibrated using standard ASTM procedures and void ratio spatial variation was calculated and represented by contour maps and histograms. The CT technique demonstrated good ability to detect specimen inhomogeneities, localization patterns, and quantifying void ratio variation within sand specimens.

Description: Morphology and structure of ZnO films deposited on (0001) sapphire and glass substrates by off-axis sputtering are investigated at various temperatures and pressures. All films show highly textured structures on glass substrates and epitaxial growth on sapphire substrates. The full width at half maximum of theta rocking curves for epitaxial films is less than 0.5 degrees. In textured films, it rises to several degrees. The trend of surface textures in films grown at low pressures is similar to those grown at high temperatures. A morphology transition from large well-defined hexagonal grains to flat surface was observed at a pressure of 50 mtorr and temperature of 550 C. The experiment results are explained by the transport behavior of depositing species.

Description: ZnO films are deposited on (0001) sapphire, (001) Si and quartz substrates using the off-axis reactive magnetron sputtering deposition. Based on film thickness measurements, three transport regions of sputtered particles are observed when films are deposited in the pressure regions of 5 mtorr - 150 mtorr. X-ray diffraction, scanning probes microscopy, and electrical measurements are also used to characterize these films. The full width at half maximum of theta rocking curves for epitaxial films is less than 0.5 deg. In textured films, it rises to several degrees. The epitaxial films deposited at high pressure reveal a flat surface with some hexagonal facets. The density of hexagonal facets decreases when the growth pressure is reduced. The resistivity of these epitaxial films also depends on the growth pressures. A relationship between the pressure effects and film properties are discussed.

Description: Two different vendor rubber formulations have been used to produce the silica-filled NBR insulators for the BSM of each of the two Solid Rocket Boosters (SRBs) on the Space Shuttle. Each cured insulator is bonded to the BSM aluminum aft closure with an epoxy adhesive, and some of the curved areas in the rubber may have significant residual stresses. A number of recently bonded NBR insulators have shown fine surface cracks, and stressed insulator areas may be aging at a faster rate than unstressed areas, thus hastening the surface cracking. Thermal analysis data on both vendor insulators by Dynamic Mechanical Analysis (DMA) through a temperature/frequency sweep from 24 to 74 C have shown a higher flexural storage modulus and Arrhenius activation energy for the stressed area than for the unstressed area. Other thermal analysis techniques are being used to study the insulator surface vs. bulk interior for better understanding this anomaly.

Description: White Hypalon paint is brush-applied as a moisture barrier coating over cork surfaces on each of the two Space Shuttle SRBS. Fine cracks have been observed in the Hypalon coating three times historically on laboratory witness panels, but never on flight hardware. Recent samples of the cracked and standard ("good") Hypalon were removed from cork surfaces and were tested by Thermal Gravimetric Analysis (TGA), Thermomechanical (TMA) and Differential Scanning Calorimetry (DSC) thermal analysis techniques. The TGA data showed that at 700 C, where only paint pigment solids remain, the cracked material had about 9 weight percent more material remaining than the standard material, probably indicating incomplete mixing of the paint before it was brush-applied to produce the cracked material. Use of the TMA film tension method showed that the average static modulus vs. temperature was about 3 to 6 times higher for the cracked material than for the standard material, indicating a much higher stiffness for the cracked Hypalon. The TMA data also showed than an increased coating thickness for the cracked Hypalon was not a factor in the anomaly.

Description: Phthalocyanine is a very stable organic material in the atmosphere and has been used in numerous applications, such as optical switching and optical storage devices. Although this material has already been discovered for several decades and has had extensive studies conducted on it, many properties still need to be better understood, for example, the mechanisms of forming different solid phases and of changing film morphology by external forces. Phthalocyanine has two preferred solid phases (alpha and beta phases) for which the crystal structures, surface morphology and optical properties are different. In order to investigate these phenomena and the relationship among them, phthalocyanine films have been synthesized by vapor deposition on quartz substrates with and without an external electrical field. Some substrates were coated with a very thin gold film for the electrical field. These films have been characterized using x-ray diffraction, scanning electron microscopy, Fourier transfer infrared spectroscopy, and Z-scan technique. The films have excellent chemical and thermal stability. However, the surface of these films grown without the electrical field shows flower-like morphology. When films are deposited under an electrical field (approximately 3000 V/cm), an aligned structure is revealed on the surface. A comparison of the structure, morphology, optical properties, and the growth mechanism for these films with and without an electrical field will be discussed.

Description: We report on the effects of melt processing temperature on structure formation in Poly(ether-ether-ketone), PEEK. Real time Small Angle X-ray Scattering, SAXS, and thermal analysis are used to follow the melting behavior after various stages of processing. Assignment of peaks to structural entities within the material, the relative perfection of the crystals, and the possibility of their reorganization, are all influenced by the melt processing history. With the advent of high intensity synchrotron sources of X-radiation, polymer scientists gain a research tool which, when used along with thermal analysis, provides additional structural information about the crystals during growth and subsequent melting. PEEK is an engineering thermoplastic polymer with a very high glass transition temperature (145 C) and crystal melting point (337 C). PEEK has been the subject of recent studies by X-ray scattering in which melt and cold crystallization were followed in real-time. X-ray scattering and thermal studies have been used to address the formation of dual endothermic response which has been variously ascribed to lamellar insertion, dual crystal populations, or melting followed by re-crystallization. Another important issue is whether all of the amorphous phase is located in interlamellar regions, or alternatively whether some is located in "pockets" away from the crystalline lamellar stacks. The interpretation of scattering from lamellar stacks varies depending upon whether such amorphous pockets are formed. Some groups believe all of the amorphous phase is interlamellar. This leads to selection of a smaller thickness for the crystals. Other groups suggest that most amorphous phase is not interlamellar, and this leads to the suggestion that the crystal thickness is larger than the amorphous layer within the stacks. To investigate these ideas, we used SAXS and Differential Scanning Calorimetry to compare results of single and dual stage melt crystallization of PEEK using a treatment scheme involving annealing/crystallization at T(sub a1) followed by annealing at T(sub a2) where either T(sub a1) 〈 T(sub a2) or T(sub a1) 〉 T(sub a2). We proposed a model to explain multiple melting endotherms in PPS, treated according to one or two-stage melt or cold crystallization. Key features of this model are that multiple endotherms: (1) are due to reorganization/recrystallization after cold crystallization; and, (2) are dominated by crystal morphology after melt crystallization at high T. In other words, multiple distinct crystal populations are formed by the latter treatment, leading to observation of multiple melting. PEEK 45OG pellets (ICI Americas) were the starting material for this study. Films were compression molded at 400 C, then quenched to ice water. Samples were heated to 375 C in a Mettler FP80 hot stage and held for three min. to erase crystal seeds before cooling them to T(sub a1) = 280 C . Samples were held at T(sub a2) for a period of time, then immediately heated to 360 C. In the second treatment samples were held at T(sub a1) = 31 C for different crystallization times t(sub c) then cooled to 295 C and held 15 min. In situ (SAXS) experiments were performed at the Brookhaven National Synchrotron Light Source with the sample located inside the Mettler hot stage. The system was equipped with a two-dimensional position sensitive detector. The sample to detector distance was 172.7 cm and the X-ray wavelength was 1.54 Angstroms. SAXS data were taken continuously during the isothermal periods and during the heating to 360 C at 5 C/min. Each SAXS scan was collected for 30 sec. Since the samples were isotropic, circular integration was used to increase the signal to noise ratio. After dual stage melt crystallization with T(sub a1) 〈 T(sub a2) the lower melting endotherm arises from holding at T(sub a1). During cooling a broad distribution of crystals forms, and the low-melting tail is perfected during T(sub al). Heating to T(sub a2) melts these imperfect crystals and allows others with greater average long spacing to form in their place. After dual stage crystallization with T(sub a1) 〉 T(sub a2), the amount of space remaining for additional growth at T(sub a2) depends upon the holding time at T(sub a1). The long period of crystals formed at T(sub a2) is smaller than that formed at T(sub a1) due to growth in a now-restricted geometry. Perfection of crystals is seen as an increase of the intensity of the population scattering at higher s, while the intensity of the population scattering at lower s stays constant. During heating from below to above the minor endotherm, we see rapid decrease of the intensity of the X-ray scattering corresponding to the population of crystals scattering in the shoulder. Another important observation is that after the sample is annealed at 295 C, the shoulder intensity is restored once again. The population scattering at higher s remains longer before it disappears in the sample treated to the second stage of melt crystallization, compared to the sample crystallized with a single stage. This could be interpreted as an effect of continued perfection of the less perfect population, which is also reflected in the increased melting temperature of the smaller endotherm as the holding time at 295 C increases. In the corresponding DSC scans we see a shift in the area and the peak temperature of the lower melting endotherm with an increase of the annealing time.

Description: ZnO is a wide-band-gap oxide material and has been used in numerous applications. It is also a good substrate for fabricating GaN-based (a blue laser candidate) devices. Off-axis sputtering technique is one of the best techniques in synthesizing oxide materials because negative ion bombardment and particle kinetic energy is greatly reduced when adatoms condense on substrates. Since the sputtered material from the target arrive on the substrate surface at a 90 deg. configuration, which differs from the normal sputtering geometry, it is expected that the film uniformity and composition distributions will be affected. However, the details of these properties and mechanisms have not been well studied. ZnO films are synthesized on (0001) sapphire and quartz substrates by off-axis sputtering deposition in various oxygen/argon mixture ratios and pressures at different temperatures. Substrates and sputtering sources are placed at three different orientations that are orthogonal to each other. The normal direction of a substrate is parallel to the gravity vector and the other is perpendicular to it. Film thickness profiles at different growth orientations are determined using a profimeter. All films grown at high temperatures have highly textured structures on quartz substrates and epitaxially grow on sapphire substrates. Because of this process, the film surface is very smooth. X-ray diffraction, scanning probe microscopy, and Fourier transfer infrared spectroscopy, and electrical measurements will be used to characterize these films. Detailed results will be discussed in the presentation.

Description: ZnO is a wide-band-gap oxide material that has many applications. A new potential application of ZnO material is for light emitting devices since its structure and electrical properties are similar to that of the GaN material (a blue laser candidate). It also is a good substrate for fabricating GaN-based devices. Off-axis sputtering technique has revealed great potential in synthesizing excellent oxide materials because the negative ion bombardment is greatly reduced when adatoms condense on substrates. The surface of films grown by off-axis sputtering will be much smoother than that produced in a regular sputtering configuration. A growth mechanism is studied by investigating the morphology and structure of ZnO films under different growth conditions and orientations. ZnO films are deposited on (0001) sapphire and quartz substrates by off- axis sputtering deposition at various oxygen/argon mixture ratios and pressures and at different temperatures. All films reveal highly textured structures on quartz substrates and epitaxial growth on sapphire substrates. Two off-axis configurations, vertical and horizontal orientations are conducted to study the process of film growth, surface morphology, and film structure. X-ray diffraction, scanning probe microscopy, and electrical measurements are used to characterize these films. Detailed results will be discussed in the presentation. Keywords: ZnO, Photonic material, Off-axis sputtering, Growth mechanism

Description: The method of seeded growth was studied for producing mondisperse colloidal silica particles. It was shown that particle size as well as weight percent solids could be controlled by using this method. The particles were characterized by transmission electron microscopy (TEM) and quasielastic light scattering (QELS). The particles were found to have a bimodal size distribution when examined by TEM. The particle size as determined by QELS was found to be roughly 10-20% larger than the particle size as determined by TEM. Furthermore, the polydispersity (standard deviation/mean particle size) as determined by QELS was found to be significantly lower than the polydispersity as determined by TEM. This underscores the importance of using TEM as a characterization technique for determining particle monodispersity. It was also noted that there was an increase in particle roughness as the weight percent of the silica particles increased and a new nucleation of particles was observed as the weight percent approached 13%. A recipe for producing monodisperse silica particles in the 150 nm size range is presented.

Description: A mold apparatus and method for resin film infusion molding including an outer mold tool having a facing sheet adapted to support a resin film and preform assembly. The facing sheet includes attachment features extending therefrom. An inner mold tool is positioned on the facing sheet to enclose the resin film and preform assembly for resin film infusion molding. The inner mold tool includes a plurality of mandrels positioned for engagement with the resin film and preform assembly. Each mandrel includes a slot formed therein. A plurality of locating bars cooperate with the slots and with the attachment features for locating the mandrels longitudinally on the outer mold tool.

Description: Miniature, lightweight, miser actuators that operate similar to biological muscles can be used to develop robotic devices with unmatched capabilities and impact many technology areas. Electroactive polymers (EAP) offer the potential to producing such actuators and their main attractive feature is their ability to induce relatively large bending or longitudinal strain. EAP actuators can change the paradigm about the complexity of robots, where robotic components such as motors, gears, bearings, and others can be eliminated with simple drive mechanisms. Generally, these materials produce a relatively low force and the applications that can be considered at the current state of the art are relatively limited. While improved material are being developed there is a need for methods to develop longitudinal actuators that can contract similar to muscles. In this study, the authors began investigating the electromechanical behavior of polymers in reaction to a complex configuration of electric fields. A computer model was used to simulate the electromechanical response. Efforts were made to develop both the material basis as well as the electromechanical modeling of the actuator.

Description: Besides the scale factor that distinguishes the various species, fundamentally biological muscles changes little between species, indicating a highly optimized system. Electroactive polymer actuators offer the closest resemblance to biological muscles, however besides the large actuation displacement these materials are falling short with regards to the actuation force. As improved materials are emerging it is becoming necessary to address key issues such as the need for effective electromechanical modeling and guiding parameters in scaling the actuators. In this paper, we will review the scaling laws for three major actuation mechanisms that are of relevance to micro electromechanical systems: electrostatic actuation, magnetic actuation, thermal bimetallic actuation, and piezoelectric actuation.

Description: This invention relates the novel diamines, the polyimide oligomers and the polyimides derived therefrom and to the method of preparing the diamines, oligomers and the polyimides. The thermoplastic polyimides derived from the aromatic diamines of this invention are characterized as having a high glass transition temperature, good mechanical properties and improved processability in the manufacture of adhesives, electronic and composite materials for use in the automotive and aerospace industry. The distinction of the novel aromatic diamines of this invention is the 2,2',6,6'-substituted biphenyl radicals which exhibit noncoplanar conformation that enhances the solubility of the diamine as well as the processability of the polyimides, while retaining a realatively high glass transition temperature and improved mechanical properties at useful temperature ranges.

Description: The importance of high fracture toughness and reliability in Si3N4, and SiC-based structural ceramics and ceramic matrix composites is reviewed. The potential of these ceramics and ceramic matrix composites for high temperature applications in defense and aerospace applications such as gas turbine engines, radomes, and other energy conversion hardware have been well recognized. Numerous investigations were pursued to improve fracture toughness and reliability by incorporating various reinforcements such as particulate-, whisker-, and continuous fiber into Si3N4 and SiC matrices. All toughening mechanisms, e.g. crack deflection, crack branching, crack bridging, etc., essentially redistribute stresses at the crack tip and increase the energy needed to propagate a crack through the composite material, thereby resulting in improved fracture toughness and reliability. Because of flaw insensitivity, continuous fiber reinforced ceramic composite (CFCC) was found to have the highest potential for higher operating temperature and longer service conditions. However, the ceramic fibers should display sufficient high temperature strength and creep resistance at service temperatures above 1000 'C. The greatest challenge to date is the development of high quality ceramic fibers with associate coatings able to maintain their high strength in oxidizing environment at high temperature. In the area of processing, critical issues are, preparation of optimum matrix precursors, precursor infiltration into fiber array, and matrix densification at a temperature, where grain crystallization and fiber degradation do not occur. A broad scope of effort is required for improved processing and properties with a better understanding of all candidate composite systems.

Description: SiO2 scale volatility and the resulting recession of SiC has been previously identified for CVD, as well as sintered, SiC and Si3N4 materials. Linear weight loss and surface recession of SiC was observed as a result of SiO2 volatility for both fuel-lean and fuel-rich gas mixtures. A strong Arrhenius temperature dependence exist and parametric studies using multiple linear regression were used to develop recession relationships as a function of e(sup -Q/RT) central dot P(sup X)V(sup y) for both lean and rich combustion conditions. Recession of 0.2 - 2.0 micron/hr is predicted for typical combustion conditions at 1200 - 1400 C, with a somewhat higher absolute recession rate and activation energy for rich combustion versus lean.

Description: Treatment of Nextel (TM) 312 in a reactive environment has been used as a low cost approach to the formation of BN on the fiber surface. Although the BN enriched surface region is extremely thin (less than 40 run), it is effective in providing debonding and composite behavior. Variation in mechanical behavior of Nextel (TM) 312/BN/Blackglas (TM) composites has been noted among panels fabricated with AF-10 cloth treated in different nitridation runs, Understanding this variation became the rationale for undertaking a detailed characterization of the nitrided fiber using field emission scanning electron microscopy, low voltage energy dispersive x-ray and Auger electron spectroscopy. Chemical composition and surface morphology are discussed in relation to observed mechanical behavior of NeXtel (TM) 312/Blackglas (TM) composites tested in bending.

Description: Ceramic thermal barrier coatings extend the operating temperature range of actively cooled gas turbine components, therefore increasing thermal efficiency. Performance and lifetime of existing ceram ic coatings are limited by spallation during heating and cooling cycles. Spallation of the ceramic is a function of its microstructure, which is determined by the deposition method. This research is investigating metalorganic chemical vapor deposition (MOCVD) of yttria stabilized zirconia to improve performance and reduce costs relative to electron beam physical vapor deposition. Coatings are deposited in an induction-heated, low-pressure reactor at 10 microns per hour. The coating's composition, structure, and response to the turbine environment will be characterized.

Description: Ceramic matrix composite (CMC) components are being designed, fabricated, and tested for a number of high temperature, high performance applications in aerospace and ground based systems. The critical need for and the role of reliable and robust databases for the design and manufacturing of ceramic matrix composites are presented. A number of issues related to engineering design, manufacturing technologies, joining, and attachment technologies, are also discussed. Examples of various ongoing activities in the area of composite databases. designing to codes and standards, and design for manufacturing are given.

Description: The method and equipment of testing continuously rolled insulation materials is presented in this paper. Testing of blanket and molded products is also facilitated. Materials are installed around a cylindrical copper sleeve using a wrapping machine. The sleeve is slid onto the vertical cold mass of the cryostat. The gap between the cold mass and the sleeve measures less than 1 mm. The cryostat apparatus is a liquid nitrogen boiloff calorimeter system that enables direct measurement of the apparent thermal conductivity (k-value) of the insulation system at any vacuum level between 5 x 10(exp -5) and 760 torr. Sensors are placed between layers of the insulation to provide complete temperature-thickness profiles. The temperatures of the cold mass (maintained at 77.8 kelvin (K)), the sleeve (cold boundary temperature (CBT)), the insulation outer surface (warm boundary temperature (WBT)), and the vacuum can (maintained at 313 K by a thermal shroud) are measured. Plots of CBT, WBT, and layer temperature profiles as functions of vacuum level show the transitions between the three dominant heat transfer modes. For this cryostat apparatus, the measureable heat gain is from 0.2 to 20 watts. The steady-state measurement of k-value is made when all temperatures and the boiloff rate are stable.

Description: Cracks and other defects in ceramic materials can be difficult or impossible to examine and photograph due to the extreme lack of contrast. A method for inspecting translucent ceramics using scattered light, also known as vicinal illumination, will be described. This method has been known in the ceramics industry for quite some time, but is not well known in the testing and failure analysis community. Electronics applications include substrates, packages, multilayer capacitors, and thin film resistors. Ceramic materials are used in electronic applications as microcircuit packages and substrates which carry signals and power between microcircuits. Fine cracks in ceramic materials can result in mechanical failures, electrical failures, and loss of hermeticity. Often, fine cracks are difficult or impossible to detect using standard nondestructive inspection techniques such as visual inspection, ultrasonic inspection, or vapor crack detection. Dye penetrant inspection is usually effective, but contaminates the part, which is unacceptable for space flight hardware. One effective nondestructive inspection method of detecting cracks involves examining the way in which light scatters through the ceramic material when viewed with a standard bright field reflected light microscope. This method, termed vicinal illumination, has been used for detecting cracks during failure analyses of several part types, and screening of space flight hardware. The technique has proven effective on several different types of ceramic materials as well. A related method for use with dark field equipment has also been used to successfully locate otherwise invisible cracks.

Description: The results of a comparative study of cryogenic insulation systems performed are presented. The key aspects of thermal insulation relative to cryogenic system design, testing, manufacturing, and maintenance are discussed. An overview of insulation development from an energy conservation perspective is given. Conventional insulation materials for cryogenic applications provide three levels of thermal conductivity. Actual thermal performance of standard multilayer insulation (MLI) is several times less than laboratory performance and often 10 times worse than ideal performance. The cost-effectiveness of the insulation system depends on thermal performance; flexibility and durability; ease of use in handling, installation, and maintenance; and overall cost including operations, maintenance, and life cycle. Results of comprehensive testing of both conventional and novel materials such as aerogel composites using cryostat boil-off methods are given. The development of efficient, robust cryogenic insulation systems that operate at a soft vacuum level is the primary focus of this paper.

Description: The microstructural properties of (Ba(0.5)Sr(0.5)TiO3) (BSTO) thin films (300, 700, and 1400 nm thick) deposited on LaAlO3 (LAO) substrates were characterized using high-resolution x-ray diffractometry. Film crystallinity was the parameter that most directly influenced tunability, and we observed that a) the crystalline quality was highest in the thinnest film and progressively degraded with increasing film thickness; and b) strain at the film/substrate interface was completely relieved via dislocation formation. Paraelectric films such as BSTO offer an attractive means of incorporating low-cost phase shifter circuitry into beam-steerable reflectarray antennas.

Description: In January 1998 during, the STS-89 mission, an eight section Russian solar array panel was retrieved after more than ten years exposure to the orbital space environment on the Russian space station Mir. Two darkened handrail samples from the Russian solar array have been evaluated for contamination: a section of a white paint covered rigid handrail and a section of woven fabric over-wrapped around a flexible handhold. The handrail samples were evaluated using optical microscopy (OM), field emission scanning electron microscopy (FESEM) and energy dispersive spectroscopy (EDS). Optical properties were also obtained. Microscopy has shown the discolored areas to have thick layers of contaminant that has crazed and spalled off in regions. Energy dispersive spectroscopy revealed that the brown contaminant is composed of oxidized silicon. No silicon was present on the unexposed fabric over-wrap, and very small amounts were present in the white paint. Therefore, the contaminant layer on both samples is attributed to silicone contamination from other spacecraft materials that have been oxidized by atomic oxygen while in orbit. A significant source of the silicone contamination appears to be from the solar array itself.

Description: The tribological properties of chemical-vapor-deposited (CVD) diamond films vary with the environment, possessing a Jekyll-and-Hyde character. CVD diamond has low coefficient of friction and high wear resistance in air but high coefficient of friction and low wear resistance in vacuum. Improving the tribological functionality of materials (such as achieving low friction and good wear resistance) was an aim of this investigation. Three studies on the surface design, surface engineering, and tribology of CVD diamond have shown that its friction and wear are significantly reduced in ultrahigh vacuum. The main criteria for judging whether diamond films are an effective wear-resistant, self-lubricating material were coefficient of friction and wear rate, which must be less than 0.1 and on the order of 10(exp 6) cu mm/N(dot)m, respectively. In the first study the presence of a thin film (less than 1 micron thick) of amorphous, nondiamond carbon (hydrogenated carbon, also called diamondlike carbon or DLC) on CVD diamond greatly decreased the coefficient of friction and the wear rate. Therefore, a thin DLC film on CVD diamond can be an effective wear-resistant, lubricating coating in ultrahigh vacuum. In the second study the presence of an amorphous, nondiamond carbon surface layer formed on CVD diamond by ion implantation significantly reduced the coefficient of friction and the wear rate in ultrahigh vacuum. Therefore, such surface layers are acceptable for effective self-lubricating, wear-resistant applications of CVD diamond. In the third study CVD diamond in contact with cubic boron nitride exhibited low coefficient of friction in ultra high vacuum. Therefore, this materials combination can provide an effective self-lubricating, wear-resistant couple in ultrahigh vacuum.

Description: Previous stressed oxidation tests of C/SiC composites at elevated temperatures (350 C to 1500 C) and sustained stresses (69 MPa and 172 MPa) have led to the development of a finite difference cracked matrix model. The times to failure in the samples suggest oxidation occurred in two kinetic regimes defined by the rate controlling mechanisms (i.e. diffusion controlled and reaction controlled kinetics). Microstructural analysis revealed preferential oxidation along as-fabricated, matrix microcracks and also suggested two regimes of oxidation kinetics dependent on the oxidation temperature. Based on experimental results, observation, and theory, a finite difference model was developed. The model simulates the diffusion of oxygen into a matrix crack bridged by carbon fibers. The model facilitates the study of the relative importance of temperature, the reaction rate constant, and the diffusion coefficient on the overall oxidation kinetics.

Description: The objective of this research and development program was to develop PbZr(1-x)Ti(x)O3 (PZT) and Pb(1-x)Ba(x)Nb2O6 (PBN) materials with large piezoelectric response which are suitable for shape control in large inflatable structures. Two approaches were to be considered: (1) direct deposition of PZT and PBN films on flexible plastic or thin metal foil substrates, and (2) deposition on Si followed by fabrication of hybrid structures on mylar or kapton. Testing in shape control concepts was carried out at JPL and based on their results, the required modifications were made in the final film compositions and deposition techniques. The program objective was to identify and then optimize piezoelectric materials for NASA shape control applications. This involved the bulk piezoelectric and photovoltaic responses and the compatibility of the thin films with appropriate substrate structures. Within the PZT system, Rockwell has achieved the highest reported piezoelectric coefficient (d(sub 33) greater than 100 pC/N) of any ceramic composition. We used this experience in piezoelectric technology to establish compositions that can effectively address the issues of this program. The performance of piezoelectric thin films depends directly on d(sub ij) and Epsilon. The challenge was to find PZT compositions that maintained high d(sub ij) and Epsilon, while also exhibiting a large photovoltaic effect and integrate thin films of this composition into the system structure necessary to meet shape control applications. During the course of this program, several PZT and PLZT compositions were identified that meet these requirements. Two such compositions were successfully used in electrical and optical actuation studies of thin film structures.

Description: This paper discusses the methodologies used for surface property measurement of thin films and coatings, lubricants, and materials in the field of tribology. Surface diagnostic techniques include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, stylus profilometry, x-ray diffraction, electron diffraction, Raman spectroscopy, Rutherford backscattering, elastic recoil spectroscopy, and tribology examination. Each diagnostic technique provides specific measurement results in its own unique way. In due course it should be possible to coordinate the different pieces of information provided by these diagnostic techniques into a coherent self-consistent description of the surface properties. Examples are given on the nature and character of thin diamond films.

Description: A vacuum ball-on-plate rolling contact tribometer was used to determine the relative lifetimes of a perfluoropolyether (Krytox 143 AC) on 440C stainless steel. The effect of mean Hertzian stresses (0.75, 1.0, 1.5 and 2.0 GPa) and the use of TiC coated balls on lubricant lifetime was studied. Other conditions included: approximately 100 rpm, approximately 50 micrograms of lubricant, an initial vacuum level of less than 1.0 x 1O(exp -8) Torr, and room temperature (approximately 23 C). increasing the mean Hertzian stress from 0.75 to 2.0 GPa results in an exponential decrease in lubricant lifetime for both material combinations. However. substituting a TiC ball for the 440C ball quadrupled lifetime at low stress levels (0.75 and 1.0 GPa) and doubled life at higher stresses (1.5 and 2.0 GPa). The reduced reactivity of the TiC surface with the PFPE lubricant is considered to be the reason for this enhancement. Decreasing lifetime with increasing stress levels correlated well with energy dissipation calculations.

Description: The friction and wear characteristics of two formulated perfluoropolyether based greases were compared to their non-additive base greases. One grease was developed for the electronics industry (designated as GXL-296A) while the other is for space applications (designated as GXL-320A). The formulated greases (GXL-296B and GXL-320B) contained a proprietary antiwear additive at an optimized concentration. Tests were conducted using a vacuum four-ball tribometer. AISI 52100 steel specimens were used for all GXL-296 tests. Both AISI 52100 steel and 440C stainless steel were tested with the GXL-320 greases. Test conditions included: a pressure less than 6.7 x 10(exp )-4 Pa, a 200N load, a sliding velocity of 28.8 mm/sec (100 rpm) and room temperature (approximately equal to 23 C). Wear rates for each grease were determined from the slope of the wear volume as a function of sliding distance. Both non-additive base greases yielded relatively high wear rates on the order of 10(exp -8) cu mm using AISI 52100 steel specimens. Formulated grease GXL-296B yielded a reduction in wear rate by a factor of approximately 21, while grease GXL-320B had a reduction of approximately 12 times. Lower wear rates (-50%) were observed with both GXL-320 greases using 440C stainless steel. Mean friction coefficients were slightly higher for both formulated greases compared to their base greases. The GXL-296 series (higher base oil viscosity) yielded much higher friction coefficients compared to their GXL-320 series (lower base oil viscosity) counterparts.

Description: Currently, most blades and vanes in the hottest section of aero gas turbine engines require some type of coating for oxidation protection. Newly developed single crystal superalloys have the mechanical potential to operate at increasingly higher component temperatures. However, at these elevated temperatures, coating/substrate interdiffusion can shorten the protective life of the coating. Diffusion barriers between overlay coatings and substrates are being examined to extend the protective life of the coating. A previously- developed finite-difference diffusion model has been modified to predict the oxidative life enhancement due to use of a diffusion barrier. The original diffusion model, designated COSIM, simulates Al diffusion in the coating to the growing oxide scale as well as Al diffusion into the substrate. The COSIM model incorporates an oxide growth and spalling model to provide the rate of Al consumption during cyclic oxidation. Coating failure is predicted when the Al concentration at the coating surface drops to a defined critical level. The modified COSIM model predicts the oxidative life of an overlay coating when a diffusion barrier is present eliminating diffusion of Al from the coating into the substrate. Both the original and the modified diffusion models have been used to predict the effectiveness of a diffusion barrier in extending the protective life of a NiCrAl overlay coating undergoing cyclic oxidation at 1100 C.

Description: The research consisted of two major parts, first modeling and simulation of the combined effects of aging and damage on polymer composites and secondly an experimental phase examining composite response at elevated temperatures, again activating both aging and damage. For the simulation, a damage model for polymeric composite laminates operating at elevated temperatures was developed. Viscoelastic behavior of the material is accounted for via the correspondence principle and a variational approach is adopted to compute the temporal stresses within the laminate. Also, the effect of physical aging on ply level stress and on overall laminate behavior is included. An important feature of the model is that damage evolution predictions for viscoelastic laminates can be made. This allows us to track the mechanical response of the laminate up to large load levels though within the confines of linear viscoelastic constitutive behavior. An experimental investigation of microcracking and physical aging effects in polymer matrix composites was also pursued. The goal of the study was to assess the impact of aging on damage accumulation, in ten-ns of microcracking, and the impact of damage on aging and viscoelastic behavior. The testing was performed both at room and elevated temperatures on [+/- 45/903](sub s) and [02/903](sub s) laminates, both containing a set of 90 deg plies centrally located to facilitate investigation of microcracking. Edge replication and X-ray-radiography were utilized to quantify damage. Sequenced creep tests were performed to characterize viscoelastic and aging parameters. Results indicate that while the aging times studied have limited ]Influence on damage evolution, elevated temperature and viscoelastic effects have a profound effect on the damage mode seen. Some results are counterintuitive, including the lower strain to failure for elevated temperature tests and the catastrophic failure mode observed for the [+/- 45/9O3](sub s), specimens. The fracture toughness for transverse cracks increases with increasing temperature for both systems: transverse cracking was completely absent prior to failure in [+/- 45/903](sub s), and was suppressed for [02/903](sub s). No significant effect of damage on aging or viscoelastic parameters was observed.

Description: Several different types of SiC fiber tows were coated with BN and composited using chemically vapor-infiltrated SiC to form single-tow minicomposites. The types of SiC fiber included Nicalon(sup TM), Hi-Nicalon(sup TM), and the new Sylramic(sup TM) polycrystalline SiC fiber. The interfacial shear stresses were determined from unload-reload tensile hysteresis-loop tests. The ultimate stress and strain properties also were determined for the minicomposites. The ultimate strengths of the newer Hi-Nicalon and Sylramic fibers were superior to that of Nicalon minicomposites with similar fiber volume fractions. The Sylramic minicomposites had the lowest strain to failure and highest interfacial shear strength, respectively, because of the high modulus of the fiber and the rough surface of this fiber type. The apparent interfacial shear strength increased as the stress increased for the Sylramic minicomposites, which also was attributed to the surface roughness of this fiber.

Description: A reverse phase High Performance Liquid Chromatographic method was developed to rapidly fingerprint a phenol-formaldehyde resole resin similar to Durite(R) SC-1008. This resin is used in the fabrication of carbon-carbon composite materials from which Space Shuttle Solid Rocket Booster nozzles are manufactured. A knowledge of resin chemistry is essential to successful composite processing and performance. The results indicate that a high quality separation of over 35 peaks in 25 minutes were obtained using a 15 cm Phenomenex LUNA C8 bonded reverse phase column, a three-way water-acetonitrile-methanol nonlinear gradient, and LTV detection at 280 nm.

Description: Heat and mass transfer in float-zone processing are strongly influenced by convective flows in the zone. They are caused by buoyancy convection, thermocapillary (Marangoni) convection, or artificial sources such as rotation and radio-frequency heating. Flows in conducting melts can be controlled by the use of magnetic fields, either by damping fluid motion with static fields or by generating a defined flow with rotating fields. The possibilities of using static and rotating magnetic fields in silicon floating-zone growth have been investigated by experiments in axial static fields up to 5 T and in transverse rotating magnetic fields up to 7.5 mT. Static fields of a few 100 mT already suppress most striations but are detrimental to the radial segregation by introducing a coring effect. A complete suppression of dopant striations caused by time-dependent thermocapillary convection and a reduction of the coring to insignificant values, combined with a shift of the axial segregation profile toward a more diffusion-limited case, is possible with static fields greater than or equal to 1 T. However, under certain conditions the use of high axial magnetic fields can lead to the appearance of a new type of pronounced dopant striations, caused by thermoelectromagnetic convection. The use of a transverse rotating magnetic field influences the microscopic segregation at quite low inductions, of the order of a few millitesla. The field shifts time- dependent flows and the resulting striation patterns from a broad range of low frequencies at high amplitudes to a few high frequencies at low amplitudes.

Description: This document, submitted by AlliedSignal Engines (AE), a division of AlliedSignal Aerospace Company, presents the program final report for the Advanced High Temperature Polymer Matrix Composites for Gas Turbine Engines Program Expansion in compliance with data requirements in the statement of work, Contract No. NAS3-97003. This document includes: 1 -Technical Summary: a) Component Design, b) Manufacturing Process Selection, c) Vendor Selection, and d) Testing Validation: 2-Program Conclusion and Perspective. Also, see the Appendix at the back of this report. This report covers the program accomplishments from December 1, 1996, to August 24, 1998. The Advanced High Temperature PMC's for Gas Turbine Engines Program Expansion was a one year long, five task technical effort aimed at designing, fabricating and testing a turbine engine component using NASA's high temperature resin system AMB-21. The fiber material chosen was graphite T650-35, 3K, 8HS with UC-309 sizing. The first four tasks included component design and manufacturing, process selection, vendor selection, component fabrication and validation testing. The final task involved monthly financial and technical reports.

Description: Life tests were conducted on instrument scanner ball bearings cleaned with 3 types of non-ozone depleting solvents and compared with those cleaned with a conventional CFC-113 (Freon) solvent. The test bearings were lubricated with the standard space oil (Bray 815Z, Fomblin Z25) and a more recent synthetic space oil (Pennzane 2001). Lives with replacement solvents equaled or exceeded those obtained with CFC-113 baseline, indicating that alternate cleaning solvents were acceptable. Pennzane lubricated bearings enjoyed a significant life advantage (〉5X) over those lubricated with Bray 815Z oil in these oscillatory gimbal bearing tests. Many of the Pennzane bearings are still exhibiting acceptable torque traces after more than 25,000 hr of test.

Description: The development of a cryogenic insulation system for operation under soft vacuum is presented in this paper. Conventional insulation materials for cryogenic applications can be divided into three levels of thermal performance, in terms of apparent thermal conductivity [k-value in milliwatt per meter-kelvin (mW/m-K)]. System k-values below 0.1 can be achieved for multilayer insulation operating at a vacuum level below 1 x 10(exp -4) torr. For fiberglass or powder operating below 1 x 10(exp -3) torr, k-values of about 2 are obtained. For foam and other materials at ambient pressure, k-values around 30 are typical. New industry and aerospace applications require a versatile, robust, low-cost thermal insulation with performance in the intermediate range. The target for the new composite insulation system is a k-value below 4.8 mW/m-K (R-30) at a soft vacuum level (from 1 to 10 torr) and boundary temperatures of approximately 77 and 293 kelvin (K). Many combinations of radiation shields, spacers, and composite materials were tested from high vacuum to ambient pressure using cryostat boiloff methods. Significant improvement over conventional systems in the soft vacuum range was demonstrated. The new layered composite insulation system was also shown to provide key benefits for high vacuum applications as well.

Description: Results of fundamental research on the tribological properties of chemical-vapor-deposited (CVD) diamond, diamondlike carbon, and cubic boron nitride films in sliding contact with CVD diamond in ultrahigh vacuum, dry nitrogen, humid air, and water are discussed. Furthermore, the actual and potential applications of the three different superhard coatings in the field of tribology technology, particularly for wear parts and tools, are reviewed.

Description: A noncontact method is described which uses atomic oxygen to remove soot and char from the surface of a painting. The atomic oxygen was generated by the dissociation of oxygen in low pressure air using radio frequency energy. The treatment, which is an oxidation process, allows control of the amount of material to be removed. The effectiveness of char removal from half of a fire-damaged oil painting was studied using reflected light measurements from selected areas of the painting and by visual and photographic observation. The atomic oxygen was able to effectively remove char and soot from the treated half of the painting. The remaining loosely bound pigment was lightly sprayed with a mist to replace the binder and then varnish was reapplied. Caution should he used when treating an untested paint medium using atomic oxygen. A representative edge or corner should he tested first in order to determine if the process would be safe for the pigments present. As more testing occurs, a greater knowledge base will be developed as to what types of paints and varnishes can or cannot be treated using this technique. With the proper precautions, atomic oxygen treatment does appear to be a technique with great potential for allowing very charred, previously unrestorable art to be salvaged.

Description: The determination of "ultra" fast fracture strengths of five silicon nitride ceramics at elevated temperatures has been made by using constant stress-rate ("dynamic fatigue") testing with a series of "ultra" fast test rates. The test material included four monolithic and one SiC whisker-reinforced composite silicon nitrides. Of the five test materials, four silicon nitrides exhibited the elevated -temperature strengths that approaches their respective room-temperature strengths at an "ultra" fast test rate of 3.3 x 10(exp 4) MPa/s. This implies that slow cracks growth responsible for elevated-temperature failure can be eliminated or minimized by using the "ultra" fast test rate. These ongoing experimental results have shed light on laying a theoretical and practical foundation on the concept and definition of elevated-temperature "inert" strength behavior of advanced ceramics.

Description: Experimental results are presented on the erosion characteristics of the polyimide Kapton H, which serves as a blanket material in solar arrays. This polymer has a number of characteristics that make it a suitable choice for both terrestrial and space applications. In this paper attention is focused on the durability of protected Kapton when exposed to atomic oxygen (AO) in a plasma asher. A strip of 0.025-mm thick Kapton film, coated on both sides with SiO2, was studied during a 1306 hour exposure. The erosion, located at defect sites in the protective coating and measured optically, is described in terms of volume loss as a function of AO fluence. Three simple geometric profiles are used to generate a useful array of cavity shapes to model erosion evolution. These models connect the volume erosion rate to the observed lateral expansion of the developing cavities via their diameters, measured adviacent to the upper and lower protective film, and fitted by least-squares regression to simple power law functions of fluence. The rationale for the choice of models is discussed. It was found that lateral growth in cavity size evolves less than linearly with fluence.

Description: This project was aimed towards a better understanding of template-directed reactions and, based on this, towards the development of efficient non-enzymatic RNA replicating systems. These systems could serve as models for the prebiotic synthesis of an RNA world. The major objectives of this project are: (a) To elucidate the mechanistic aspects of template-directed (TD) chemistry and (b) to identify active boundary regions, or conditions, environmental and other, that favor "organized chemistry" and stereo-selective polymerization of nucleotides. "Organized chemistry" may lead to enhanced polymerization efficiency which in turn is expected to facilitate the road towards a self-replicating chemical system based on all four nucleic acid bases.

Description: The exposure of silicones to atomic oxygen in low Earth orbit causes oxidation of the surface, resulting in conversion of silicone to silica. This chemical conversion increases the elastic modulus of the surface and initiates the development of a tensile strain. Ultimately, with sufficient exposure, tensile strain leads to cracking of the surface enabling the underlying unexposed silicone to be converted to silica resulting in additional depth and extent of cracking. The use of silicone coatings for the protection of materials from atomic oxygen attack is limited because of the eventual exposure of underlying unprotected polymeric material due to deep tensile stress cracking of the oxidized silicone. The use of moderate to high volatility silicones in low Earth orbit has resulted in a silicone contamination arrival at surfaces which are simultaneously being bombarded with atomic oxygen, thus leading to conversion of the silicone contaminant to silica. As a result of these processes, a gradual accumulation of contamination occurs leading to deposits which at times have been up to several microns thick (as in the case of a Mir solar array after 10 years in space). The contamination species typically consist of silicon, oxygen and carbon. which in the synergistic environment of atomic oxygen and UV radiation leads to increased solar absorptance and reduced solar transmittance. A comparison of the results of atomic oxygen interaction with silicones and silicone contamination will be presented based on the LDEF, EOIM-111, Offeq-3 spacecraft and Mir solar array in-space results. The design of a contamination pin-hole camera space experiment which uses atomic oxygen to produce an image of the sources of silicone contamination will also be presented.

Description: The objective of this research and development program was to develop PbZr(1-x)Ti(x)O3 (PZT) and Pb(1-x)Ba(x)Nb2O6 (PBN) materials with large piezoelectric response which are suitable for shape control in large inflatable structures. Two approaches were to be considered: (1) direct deposition of PZT and PBN films on flexible plastic or thin metal foil substrates, and (2) deposition on Si followed by fabrication of hybrid structures on mylar or kapton. Testing in shape control concepts was carried out at JPL and based on their results, the required modifications were made in the final film compositions and deposition techniques. The program objective was to identify and then optimize piezoelectric materials for NASA shape control applications. This involved the bulk piezoelectric and photovoltaic responses and the compatibility of the thin films with appropriate substrate structures. Within the PZT system, Rockwell has achieved the highest reported piezoelectric coefficient (d(sub 33) greater than 100 pC/N) of any ceramic composition. We used this experience in piezoelectric technology to establish compositions that can effectively address the issues of this program. The performance of piezoelectric thin films depends directly on d(sub ij) and epsilin. The challenge was to find PZT compositions that maintained high d(sub ij) and epsilon, while also exhibiting a large photovoltaic effect and integrate thin films of this composition into the system structure necessary to meet shape control applications. During the course of this program, several PZT and PLZT compositions were identified that meet these requirements. Two such compositions were successfully used in electrical and optical actuation studies of thin film structures.

Description: The central theme of this research is the application of carboxylate-alumoxane nanoparticles as precursors to thermally protective coatings for high temperature polymer composites. In addition, we will investigate the application of carboxylate-alumoxane nanoparticle as a component to polymer composites. The objective of this research was the high temperature protection of polymer composites via novel chemistry. The significance of this research is the development of a low cost and highly flexible synthetic methodology, with a compatible processing technique, for the fabrication of high temperature polymer composites. We proposed to accomplish this broad goal through the use of a class of ceramic precursor material, alumoxanes. Alumoxanes are nano-particles with a boehmite-like structure and an organic periphery. The technical goals of this program are to prepare and evaluate water soluble carboxylate-alumoxane for the preparation of ceramic coatings on polymer substrates. Our proposed approach is attractive since proof of concept has been demonstrated under the NRA 96-LeRC-1 Technology for Advanced High Temperature Gas Turbine Engines, HITEMP Program. For example, carbon and Kevlar(tm) fibers and matting have been successfully coated with ceramic thermally protective layers.

Description: Magnetorheological (MR) suspensions are composed of colloidal particles which acquire dipole moments when subjected to an external magnetic field. At sufficient field strengths and concentrations, the dipolar particles rapidly aggregate to form long chains. Subsequent lateral cross-linking of the dipolar chains is responsible for a rapid liquid-to-solid-like rheological transition. The unique, magnetically-activated rheological properties of MR suspensions make them ideal for interfacing mechanical systems to electronic controls. Additionally, the ability to experimentally probe colloidal suspensions interacting through tunable anisotropic potentials is of fundamental interest. Our current experimental work has focused on understanding the fluctuations of dipolar chains. It has been proposed by Halsey and Toor (HT) that the strong Landau-Peierls thermal fluctuations of dipolar chains could be responsible for long-range attractions between chains. Such interactions will govern the long-time relaxation of MR suspensions. We have synthesized monodisperse neutrally buoyant MR suspensions by density matching stabilized ferrofluid emulsion droplets with D2O. This allows us to probe the dynamics of the dipolar chains using light scattering without gravitational, interfacial, and polydispersity effects to resolve the short-wavelength dynamics of the dipolar chains. We used diffusing wave spectroscopy to measure these dynamics. The particle displacements at short times that show an independence to the field strength, but at long times exhibit a constrained, sub-diffusive motion that slows as the dipole strength is increased. The experiments are in good qualitative agreement with Brownian dynamics simulations of dipolar chains. Although there have been several important and detailed studies of the structure and interactions in MR suspensions, there has not been conclusive evidence that supports or contradicts the HT model prediction that long-range interactions exist between fluctuating chains of dipolar particles. Resolving this issue would contribute greatly to the understanding of these interesting and important materials. We have begun to test the predictions of the HT model by both examining the dynamics of individual chains and by measuring the forces between dipolar chains directly to accurately and quantitatively assess the interactions that they experience. To do so, we employ optical trapping techniques and video-microscopy to manipulate and observe our samples on the microscopic level. With these techniques, it is possible to observe chains that are fluctuating freely in three-dimensions, independent of interfacial effects. More importantly, we are able to controllably observe the interactions of two chains at various separations to measure the force-distance profile. The techniques also allow us to study the mechanical properties of individual chains and chain clusters. Our work to this point has focused on reversibly-formed dipolar chains due to field induced dipoles where the combination of this chaining, the dipolar forces, and the hydrodynamic interactions that dictate the rheology of the suspensions. One can envision, however, many situations where optical, electronic, or rheological behavior may be optimized with magneto-responsive anisotropic particles. Chains of polarizable particles may have the best properties as they can coil and flex in the absence of a field and stiffen and orient when a field is applied. We have recently demonstrated a synthesis of stable, permanent paramagnetic chains by both covalently and physically linking paramagnetic colloidal particles. The method employed allows us to create monodisperse chains of controlled length. We observed the stability, field-alignment, and rigidity of this new class of materials. The chains may exhibit unique rheological properties in an applied magnetic field over isotropic suspensions of paramagnetic particles. They are also useful rheological models as bead-spring systems. These chains form the basis for our current experiments with optical traps.

Description: Research conducted at NASA Ames Research Center has shown that the color-change response of a shear-sensitive liquid crystal coating (SSLCC) to aerodynamic shear depends on both the magnitude of the local shear vector and its direction relative to the observer's in-plane line of sight. In conventional applications, the surface of the SSLCC exposed to aerodynamic shear is illuminated with white light from the normal direction and observed from an oblique above-plane view angle of order 30 deg. In this top-light/top-view mode, shear vectors with components directed away from the observer cause the SSLCC to exhibit color-change responses. At any surface point, the maximum color change (measured from the no-shear red or orange color) always occurs when the local vector is aligned with, and directed away from, the observer. The magnitude of the color change at this vector-observer-aligned orientation scales directly with shear stress magnitude. Conversely, any surface point exposed to a shear vector with a component directed toward the observer exhibits a non-color-change response, always characterized by a rusty-red or brown color, independent of both shear magnitude and direction. These unique, highly directional color-change responses of SSLCCs to aerodynamic shear allow for the full-surface visualization and measurement of continuous shear stress vector distributions. The objective of the present research was to investigate application of the SSLCC method through a transparent test surface. In this new back-light/back-view mode, the exposed surface of the SSLCC would be subjected to aerodynamic shear stress while the contact surface between the SSLCC and the solid, transparent wall would be illuminated and viewed in the same geometrical arrangement as applied in conventional applications. It was unknown at the outset whether or not color-change responses would be observable from the contact surface of the SSLCC, and, if seen, how these color-change responses might relate to those observed in standard practice.

Description: Ceramics are protected from high temperature degradation, including high temperature, oxidative, aeroconvective degradation by a high temperature and oxidation resistant coating of a room temperature curing, hydrolyzed and partially condensed liquid polyorganosiloxane to the surface of the ceramic. The liquid polyorganosiloxane is formed by the hydrolysis and partial condensation of an alkyltrialkoxysilane with water or a mixture of an alkyltrialkoxysilane and a dialkyldialkoxysilane with water. The liquid polyorganosiloxane cures at room temperature on the surface of the ceramic to form a hard, protective, solid coating which forms a high temperature environment, and is also used as an adhesive for adhering a repair plug in major damage to the ceramic. This has been found useful for protecting and repairing porous, rigid ceramics of a type used on reentry space vehicles.

Description: A shaped article composed of an aromatic polyimide has a hollow, essentially spherical structure and a particle size of about 100 to about 1500 microns, a density of about I to about 6 pounds/ft3 and a volume change of 1 to about 20% by a pressure treatment of 30 psi for 10 minutes at room temperature. A syntactic foam, made of a multiplicity of the shaped articles which are bounded together by a matrix resin to form an integral composite structure, has a density of about 3 to about 30 pounds/cu ft and a compression strength of about 100 to about 1400 pounds/sq in.

Description: A thermally stable, piezoelectric and pyroelectric polymeric substrate was prepared. This thermally stable, piezoelectric and pyroelectric polymeric substrate may be used to prepare electromechanical transducers, thermomechanical transducers, accelerometers, acoustic sensors, infrared sensors, pressure sensors, vibration sensors, impact sensors. in-situ temperature sensors, in-situ stress/strain sensors, micro actuators, switches, adjustable fresnel lenses, speakers, tactile sensors, weather sensors, micro positioners, ultrasonic devices, power generators, tunable reflectors, microphones, and hydrophones. The process for preparing these polymeric substrates includes: providing a polymeric substrate having a softening temperature greater than 100 C; depositing a metal electrode material onto the polymer film; attaching a plurality of electrical leads to the metal electrode coated polymeric substrate; heating the metal electrode coated polymeric substrate in a low dielectric medium: applying a voltage to the heated metal electrode coated polymeric substrate to induce polarization; and cooling the polarized metal electrode coated polymeric electrode while maintaining a constant voltage.

Description: Fully-cured aromatic polyimides were prepared from various combinations of five dianhydrides and six diamines. When heated progressively under constant load, most of the films elongated rapidly near their glass transition temperatures. In about half of the nineteen materials, the strain was self-limiting - a possible indication of strain-induced crystallinity. The presence of crystallinity was established unambiguously for one material.

Description: Four research areas at the NASA Glenn Research Center involving the tribology of space mechanisms are highlighted. These areas include: soluble boundary lubrication additives for perfluoropolyether liquid lubricants, a Pennzane dewetting phenomenon, the effect of ODC-free bearing cleaning processes on bearing lifetimes and the development of a new class of liquid lubricants based on silahydrocarbons.

Description: To evaluate commercially developed solid film lubricants for aerospace bearing applications, we investigated the friction and wear behavior of bonded molybdenum disulfide (MoS2), magnetron-sputtered MoS2 and ion-plated silver films in sliding contact with 6-mm-diameter American Iron and Steel Institute (AISI) 440 C stainless steel balls. Unidirectional sliding friction experiments were conducted with a load of 5.9 N (600 g), a mean Herizian contact pressure of 0.79 GPa maximum 1.19 GPa), and a sliding velocity of 0.2 m/s at room temperature in three environments: ultrahigh vacuum (7x10 (exp -7Pa)), humid air (approx. 20 percent humidity), and dry nitrogen (less than 1 percent humidity). The resultant films were characterized by scanning electron microscopy, energy-dispersive x-ray spectroscopy, and surface profilometry. Marked differences in friction and wear resulted front the environmental conditions and the film materials. The main criteria for judging the performance were coefficient of friction and wear rate, which had to be less than 0.3 and on the order of 10 (exp -6mm exp 3/Nm or less), respectively. The bonded MoS2 and magnetron-sputtered MoS2 films met the criteria in all three environments. Also, the wear rates of the counterpart AISI 440 C stainless steel balls met that criterion in all three environments. The ion-plated silver films met the criteria only in ultrahigh vacuum. In ultrahigh vacuum the bonded MoS2 films were superior. In humid air the bonded MoS2 films had higher coefficient of friction and shorter wear life than did the magnetron-sputtered MoS2 films. The ion-plated silver films had a high coefficient of friction in humid air but relatively low coefficients of friction in the nonoxidative environments. Adhesion and plastic deformation played important roles in all three environments. All sliding involved adhesive transfer of materials.

Description: Perovskite Ba(0.5)SR(0.5)TiO3 thin films have been synthesized on (001) LaAl03 substrates by pulsed laser ablation. Extensive X-ray diffraction, rocking curve, and pole-figure studies suggest that the films are c-axis oriented and exhibit good in-plane relationship of 〈100〉(sub BSTO)//〈100〉(sub LAO). Rutherford Backscattering Spectrometry studies indicate that the epitaxial films have excellent crystalline quality with an ion beam minimum yield chi(sub min) Of only 2.6 %. The dielectric property measurements by the interdigital technique at 1 MHz show room temperature values of the relative dielectric constant, epsilon(sub r), and loss tangent, tan(sub delta), of 1430 and 0.007 with no bias, and 960 and 0.001 with 35 V bias, respectively. The obtained data suggest that the as-grown Ba(0.5)SR(0.5)TiO3 films can be used for development of room-temperature high-frequency tunable elements.

Description: A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a percursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon, metal, chloride, and oxygen. This intermediary product can be further processed by direct exposure to carbonate solutions to form a second intermediary product comprising carbon, metal carbonate, and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide; b) in an inert environment to produce metal oxide on carbon substrate; c) in a reducing environment to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

Description: There are a select number of polyimides which are soluble in organic media. Incorporation of hexafluoroisopropylidene groups is a route to achieving solubility. Such fluorinated polyimides have desirable properties for processing and electronic purposes; however, they often have linear coefficients of thermal expansion (CTE) which are well above those for metals and inorganic oxides or ceramics with which they might be bonded. We have developed a synthesis of composite inorganic-polyimide films using diaquotris(2,4-pentane-dionato)lanthanam(III) as the inorganic precursor and two soluble polyimides formed from 2,2-bis(3,4- dicarboxyphenyl)hexafluoro-propane (6FDA) and 1,3-bis(3-aminophenoxy)benzene (APB) or 2,2-bis[4-(4-aminophenoxy)phenyllhexafluoropropane (4-BDAF). A primary goal of our work was to control the linear CTE in these fluorinated polymer composites without adversely affecting mechanical or other thermal properties.

Description: Luminescent molecular probes imbedded in a polymer binder form a temperature or pressure paint. On excitation by light of the proper wavelength, the luminescence, which is quenched either thermally or by oxygen, is detected by a camera or photodetector. From the detected luminescent intensity, temperature and pressure can be determined. The basic photophysics, calibration, accuracy and time response of luminescent paints is described followed by applications in wind tunnels and in rotating machinery.

Description: An overview of the piezoelectric activity in amorphous piezoelectric polymers is presented. The criteria required to render a polymer piezoelectric are discussed. Although piezoelectricity is a coupling between mechanical and electrical properties, most research has concentrated on the electrical properties of potentially piezoelectric polymers. In this work, we present comparative mechanical data as a function of temperature and offer a summary of polarization and electromechanical properties for each of the polymers considered.