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NASA NTRS2004

PETI-298 Prepared by Microwave Synthesis: Neat Resin and Composite Properties

PETI-298 is a high temperature/high performance matrix resin that is processable into composites by resin transfer molding (RTM), resin infusion and vacuum assisted RTM techniques. It is typically synthesized in a polar aprotic solvent from the reaction of an aromatic anhydride and a combination of diamines and endcapped with phenylethynylphthalic anhydride. Microwave synthesis of PETI-298 was investigated as a means to eliminate solvent and decrease reaction time. The monomers were manually mixed and placed in a microwave oven for various times to determine optimum reaction conditions. The synthetic process was subsequently scaled-up to 330g. Three batches were synthesized and combined to give 1 kg of material that was characterized for thermal and rheological properties and compared to PETI-298 prepared by the classic solution based synthetic method. The microwave synthesized PETI-298 was subsequently used to fabricate flat laminates on T650 carbon fabric by RTM. The composite panels were analyzed and mechanical properties determined and compared with those fabricated from PETI-298 prepared by the classic solution method. The microwave synthesis process and characterization of neat resin and carbon fiber reinforced composites fabricated by RTM will be presented. KEY WORDS: Resin Transfer Molding, High Temperature Polymers, Phenylethynyl Terminated Imides, Microwave Synthesis

Smith, Joseph G.↗

NASA NTRS2001

Purification Procedures for Single-Wall Carbon Nanotubes

This report summarizes the comparison of a variety of procedures used to purify carbon nanotubes. Carbon nanotube material is produced by the arc process and laser oven process. Most of the procedures are tested using laser-grown, single-wall nanotube (SWNT) material. The material is characterized at each step of the purification procedures by using different techniques including scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), Raman, X-ray diffractometry (XRD), thermogravimetric analysis (TGA), nuclear magnetic resonance (NMR), and high-performance liquid chromatography (HPLC). The identified impurities are amorphous and graphitic carbon, catalyst particle aggregates, fullerenes, and hydrocarbons. Solvent extraction and low-temperature annealing are used to reduce the amount of volatile hydrocarbons and dissolve fullerenes. Metal catalysts and amorphous as well as graphitic carbon are oxidized by reflux in acids including HCl, HNO3 and HF and other oxidizers such as H2O2. High-temperature annealing in vacuum and in inert atmosphere helps to improve the quality of SWNTs by increasing crystallinity and reducing intercalation.

Gorelik, Olga P.↗

NASA NTRS2005

Application of Ultrasonic Guided Waves for Evaluating Aging Wire Insulation

Aging wiring has become a critical issue to the aerospace and aircraft industries due to Shuttle and aircraft incidents. The problem is that over time the insulation on wire becomes brittle and cracks. This exposes the underlying conductive wire to the potential for short circuits and fire. Popular methods of monitoring aging wire problems focuses on applying electrical sensing techniques that are sensitive to the conductor's condition, but not very sensitive to the wire insulation's condition. Measurement of wire insulation stiffness and ultrasonic properties by ultrasonic guided waves is being examined. Experimental measurements showed that the lowest order extensional mode could be sensitive to stiffness changes in the wire insulation. To test this theory conventional wire samples were heat damaged in an oven, in a range of heating conditions. The samples were 12, 16, and 20 gauge and the heat damage introduced material changes in the wire insulation that made the originally flexible insulation brittle and darker in color. Results showed that extensional mode phase velocity increased for the samples that were exposed to heat for longer duration.

Anastasi, Robert F.↗

NASA NTRS2005

Mars Geochemical Instrument (MarGI): An instrument for the analysis of the Martian surface and the search for evidence of life

The Mars Geochemical Instrument, MarGI, was developed to provide a comprehensive analysis of the rocks and surface material on Mars. The instrument combines Differential Thermal Analysis (DTA) with miniature Gas Chromatography-Ion Mobility Spectrometry (GC-IMS) to identify minerals, the presence and state of water, and organic compounds. Miniature pyrolysis ovens are used to both, conduct DTA analysis of soil or crushed rocks samples, and pyrolyze the samples at temperatures up to 1000 degrees C for GC-IMS analysis of the released gases. This combination of analytical processes and techniques, which can characterize the mineralogy of the rocks and soil, and identify and quantify volatiles released during pyrolysis, has applications across a wide range of target sites including comets, planets, asteroids, and moons such as Titan and Europa. The MarGI analytical approach evolved from the Cometary Ice and Dust Experiment (CIDEX) selected to fly on the Comet Rendezvous Asteroid Flyby Mission (CRAF).

Kojiro, Daniel R.↗

NASA NTRS2004

Reducing the Cation Exchange Capacity of Lithium Clay to Form Better Dispersed Polymer-Clay Nanocomposites

Polymer-clay nanocomposites have exhibited superior strength and thermo- oxidative properties as compared to pure polymers for use in air and space craft; however, there has often been difficulty completely dispersing the clay within the matrices of the polymer. In order to improve this process, the cation exchange capacity of lithium clay is first lowered using twenty-four hour heat treatments of no heat, 130 C, 150 C, or 170 C to fixate the lithium ions within the clay layers so that they are unexchangeable. Generally, higher temperatures have generated lower cation exchange capacities. An ion exchange involving dodecylamine, octadecylamine, or dimethyl benzidine (DMBZ) is then employed to actually expand the clay galleries. X-ray diffraction and transmission electron microscopy can be used to determine whether the clay has been successfully exfoliated. Finally, resins of DMBZ with clay are then pressed into disks for characterization using dynamic mechanical analyzer and oven- aging techniques in order to evaluate their glass transition, modulus strength, and thermal-oxidative stability in comparison to neat DMBZ. In the future, they may also be tested as composites for flexural and laminar shear strength.

Liang, Maggie↗

NASA NTRS2005

Determination of Interlaminar Toughness of IM7/977-2 Composites at Temperature Extremes and Different Thicknesses

Composite materials are being used in the aerospace industry as a means of reducing vehicle weight. In particular, polymer matrix composites (PMC) are good candidates due to their high strength-to-weight and high stiffness-to-weight ratios. Future reusable space launch vehicles and space exploration structures will need advanced light weight composites in order to minimize vehicle weight while demonstrating robustness and durability, guaranteeing high factors of safety. In particular, the implementation of composite cryogenic propellant fuel tanks (cryotanks) for future reusable launch vehicles (RLVs) could greatly reduce the vehicle's weight versus identically sized cryotanks constructed of metallic materials. One candidate composite material for future cryotank designs is IM7/977-2, which is a graphite/epoxy system. A successful candidate must demonstrate reasonable structural properties over a wide range of temperatures. Since the matrix material is normally the weak link in the composite, tests that emphasize matrix-dominated behavior need to be conducted. Therefore, the objective of this work is to determine the mode I interlaminar fracture toughness of "unidirectional" 8-ply and 16-ply IM7/977-2 through experimental testing. Tests were performed at -196 degrees Celsius (-320 degrees Fahrenheit), 22 degrees Celsius (72 degrees Fahrenheit), 93 degrees Celsius (200 degrees Fahrenheit) and 160 degrees C (320 degrees Fahrenheit). Low temperature testing was completed while the specimen was submerged in a liquid nitrogen bath. High temperature testing was completed in a temperature-controlled oven.

Johnson, W. S.↗

NASA NTRS2004

High-Temperature Probe Station Developed to Characterize Microwave Devices Through 500 C

A photograph and a block diagram of the high-temperature probe station are shown. The system consists of the ceramic heater mounted on a NASA shuttle tile insulator, a direct current power supply, a personal-computer-based data acquisition and temperature controller, microwave probes, a microscope, and a network analyzer. The ability to perform microwave tests at high temperatures is becoming necessary. There is now a need for sensors and communication circuits that can operate at 500 C and above for aircraft engine development and monitoring during flight. To address this need, researchers have fabricated devices using wide bandgap semiconductors such as SiC with targeted operating temperatures of 500 to 600 C. However, the microwave properties of these devices often change drastically with temperature, so any designs that are intended to be used in such an environment must be characterized at high temperatures. For some reliability, lifetime, and direct-current testing, the device under test can be packaged and characterized in an oven. However, for RF and microwave measurements, it is usually not possible to establish a calibrated reference plane at the device terminals within a package. In addition, the characteristics of the package would vary over a 500 C temperature range, and this would have to be accounted for when the data were analyzed. A high temperature probe station allows circuits and devices to be characterized through on wafer measurements across a broad temperature range with known reference plane. The conventional, commercially available thermal wafer-probe stations that are used to evaluate microwave devices across a controlled temperature range have a typical upper limit of 200 C. Standalone thermal heating chucks are available with an extended upper temperature range of 300 to 400 C. To effectively characterize devices at temperatures up to and surpassing 500 C, Glenn researchers developed a custom probe station. In the past, custom probe stations have been developed to test devices under other extreme environments, such as cryogenic temperatures as low as 37 K. Similarly, this custom probe station was specifically modified for high-temperature use. It allows devices to be measured quickly and flexibly, without the use of wire bonds and test fixtures. The probe station is shown making scattering parameter measurements from 1 to 50 GHz with a Hewlett-Packard 8510C Network Analyzer. There is a half-wafer of silicon directly on top of the heater to provide a uniform heated platform for our sample. A quarter wafer of silicon carbide forms the substrate for our test circuit of several transmission lines.

Downey, Alan N.↗

NASA NTRS2003

Collaboration of the NASA Glenn Research Center and Rolls-Royce Developed Thin Film Multilayered Dielectrics for Harsh Environments

The use of thin films to electrically insulate thin film sensors on engine components minimizes the intrusiveness of the sensors and allows a more accurate measurement of the environment. A variety of insulating films were investigated for preventing electrical shorting caused by insulator failure between the sensor and the component. By alternating layers of sputtered high-temperature ceramics, a sequence of insulating layers was devised that (1) prevents pinholes from forming completely through the insulator and (2) maintains high electrical resistivity at high temperatures. The total thickness is only a fraction of that needed for conventional insulating techniques. The Sensors and Electronics Technology Branch of the NASA Glenn Research Center has an in-house effort to develop thin film sensors for surface measurement in propulsion system research. Thin film sensors do not require special machining of the components on which they are mounted, and they are considerably thinner (less than 10 mm thick) than wire or foil sensors. The thin film sensors are thus much less disturbing to the operating environment and have a minimal impact on the physical characteristics of the supporting component. To further this research, NASA Glenn and Rolls-Royce (Derby, UK), with assistance from the Ohio Aerospace Institute (OAI) and the Akima Corporation, pursued a joint investigation using multilayered thin film dielectrics as a reliable insulator in harsh environments. The use of a multilayered scheme is thought to be promising for the fabrication of electrically insulating thin films. A major cause of conduction in thin film dielectrics is the presence of defects, such as pinholes, that propagate through the film to the underlying substrate surface. By alternating the insulating material, each new growth pattern would deviate from the previous one, eliminating direct pathways for conduction to the substrate. The film depositions and testing were conducted in the Instrument Research Laboratory at Glenn. The multilayered insulator test samples were made from alumina and stainless steel shims that were first covered with a sputtered underlayer of either yttria-stabilized zirconia or chromium carbide, and then overcoated with a sputtered top layer of alumina. An example of a test sample is shown in the following photograph. Each multilayered insulator sample was 5 mm thick, at least an order of magnitude thinner than conventional insulators. The insulating properties of the samples were tested in a high-temperature air oven to determine their suitability. The multilayer insulators tested showed a stabilized film at temperatures in excess of 800 C (1472 F). The underlying materials in these multilayers allow thermal expansion stresses produced during the heating to be graded. The chromium carbide-alumina multilayer had the best adhesion at high temperatures, presumably from the induced chemical bonding between the substrate and the chromium carbide underlayer. However, the zirconia-alumina multilayer proved to have slightly better insulating properties when adhering. The application of the zirconia-alumina insulator has been demonstrated on a nickel-alloy fan blade, as shown. The insulators using thin film sensors still need to be tested in a relevant high-temperature combustion environment.

Wrbanek, John D.↗

NASA NTRS2003

Field Effects of Buoyancy on a Premixed Turbulent Flame Studied by Particle Image Velocimetry

Typical laboratory flames for the scientific investigation of flame/turbulence interactions are prone to buoyancy effects. Buoyancy acts on these open flame systems and provides upstream feedbacks that control the global flame properties as well as local turbulence/flame interactions. Consequently the flame structures, stabilization limits, and turbulent reaction rates are directly or indirectly coupled with buoyancy. The objective of this study is to characterize the differences between premixed turbulent flames pointing upwards (1g), pointing downwards (-1g), and in microgravity (mg). The configuration is an inverted conical flame stabilized by a small cone-shaped bluff body that we call CLEAN Flames (Cone-Stabilized Lean Flames). We use two laser diagnostics to capture the velocity and scalar fields. Particle image velocimetry (PIV) measures the mean and root mean square velocities and planar imaging by the flame fronts method outlines the flame wrinkle topology. The results were obtained under typical conditions of small domestic heating systems such as water heaters, ovens, and furnaces. Significant differences between the 1g and -1g flames point to the need for including buoyancy contributions in theoretical and numerical calculations. In Earth gravity, there is a complex coupling of buoyancy with the turbulent flow and heat release in the flame. An investigation of buoyancy-free flames in microgravity will provide the key to discern gravity contributions. Data obtained in microgravity flames will provide the benchmark for interpreting and analyzing 1g and -1g flame results.

Cheng, Robert K.↗

NASA NTRS2004

PS300 Tribomaterials Evaluated at 6500C by Bushing Test Rig

A new facility has been developed to test the tribological behavior (friction and wear) of PS300 solid lubricant bushings at high temperatures. PS300 is a commercially available solid lubricant invented at the NASA Glenn Research Center. It can be prepared as a plasma spray coating or as a free-standing powder metallurgy component, designated PM300. PS300 and PM300 composites are designed to lubricate sliding components at temperatures above the capability of today's best oils, greases, and solid lubricants. One of the primary applications being pursued for PM300 is the development of bushings for use in high-temperature machinery. Examples include inlet guide vane bushings for gas turbines and conveyors, and bearings for industrial furnaces and ovens. Encouraging preliminary field trials indicate that PS300 and PM300 lubricant materials have been commercialized successfully in several industrial applications. However, the lack of laboratory performance data has hindered further commercialization especially for new applications that differ significantly from the established experience base. The purpose of the newly developed bushing test rig will be to determine the performance characteristics of PM300, and other materials, under conditions closely matching intended applications. The data will be used to determine engineering friction and wear rates and to estimate the life expectancy of bushings for new applications. In the new rig, the bushing is loaded against a rotating shaft inside a furnace enclosure (see the preceding photograph). Loads can vary from 5 to 200 N, speeds from 1 to 400 rpm, and temperatures from 25 to 800 C. Furnace temperature, bushing temperature, shaft speed, and torque are monitored during the test, and wear of both the bushing and the shaft is measured after testing is completed. Initially, PM300 bushings will be evaluated and compared with lower temperature, traditional bushing materials like graphite and porous bronze. The baseline PM304 composition is 60 wt% NiCr (a binder), 20 wt% Cr2O3 (a hardener), 10 wt% BaF2/CaF2 (a high-temperature lubricant), and 10 wt% Ag (a low-temperature lubricant). Future research efforts will include determining the effects of load, sliding speed, and temperature on tribological performance and, possibly, tailoring composition for specific applications. We expect that the availability of measured performance data will enhance the market penetration of PM300 technology.

Striebing, Donald R.↗

NASA NTRS2005

Higher Order Chemistry Models in the CFD Simulation of Laser-Ablated Carbon Plumes

Production of single-walled carbon nanotubes (SWNT) has taken place for a number of years and by a variety of methods such as laser ablation, chemical vapor deposition, and arc-jet ablation. Yet, little is actually understood about the exact chemical kinetics and processes that occur in SWNT formation. In recent time, NASA Johnson Space Center has devoted a considerable effort to the experimental evaluation of the laser ablation production process for SWNT originally developed at Rice University. To fully understand the nature of the laser ablation process it is necessary to understand the development of the carbon plume dynamics within the laser ablation oven. The present work is a continuation of previous studies into the efforts to model plume dynamics using computational fluid dynamics (CFD). The ultimate goal of the work is to improve understanding of the laser ablation process, and through that improved understanding, refine the laser ablation production of SWNT.

Greendyke, R. B.↗

NASA NTRS2006

Carbon Nanotube Activities at NASA-Johnson Space Center

Research activities on carbon nanotubes at NASA-Johnson Space Center include production, purification, characterization and their applications for human space flight. In-situ diagnostics during nanotube production by laser oven process include collection of spatial and temporal data of passive emission and laser induced fluorescence from C2, C3 and Nickel atoms in the plume. Details of the results from the "parametric study" of the pulsed laser ablation process indicate the effect of production parameters including temperature, buffer gas, flow rate, pressure, and laser fluence. Improvement of the purity by a variety of steps in the purification process is monitored by characterization techniques including SEM, TEM, Raman, UV-VIS-NIR and TGA. A recently established NASA-JSC protocol for SWCNT characterization is undergoing revision with feedback from nanotube community. Efforts at JSC over the past five years in composites have centered on structural polymednanotube systems. Recent activities broadened this focus to multifunctional materials, supercapacitors, fuel cells, regenerable CO2 absorbers, electromagnetic shielding, radiation dosimetry and thermal management systems of interest for human space flight. Preliminary tests indicate improvement of performance in most of these applications because of the large surface area as well as high electrical and thermal conductivity exhibited by SWCNTs.

Arepalli, Sivaram↗

NASA NTRS2006

Survey of Dust Issues for Lunar Seals and the RESOLVE Project

Lunar dust poses a technical challenge for sealing applications on the moon. A survey of seals used in Apollo lunar missions is presented as well as lunar soil characteristics and a description of the lunar environment. Seal requirements and technical challenges for the volatiles characterization oven and hydrogen reduction reaction chamber of the RESOLVE project are discussed. The purpose of the RESOLVE project is to find water or ice in lunar soil and demonstrate the ability to produce water, and hence oxygen and hydrogen, from lunar regolith for life support and propellants.

Proctor, Margaret P.↗

NASA NTRS2004

Examination of B. subtilis var. niger Spore Killing by Dry Heat Methods

Dry heat microbial reduction is the only NASA approved sterilization method to reduce the microbial bioburden on space-flight hardware prior to launch. Reduction of the microbial bioburden on spacecraft is necessary to meet planetary protection requirements specific for the mission. Microbial bioburden reduction also occurs if a spacecraft enters a planetary atmosphere (e.g., Mars) and is heated due to frictional forces. Temperatures reached during atmospheric entry events (>200 C) are sufficient to damage or destroy flight hardware and also kill microbial spores that reside on the in-bound spacecraft. The goal of this research is to determine the survival rates of bacterial spores when they are subjected to conditions similar to those the spacecraft would encounter (i.e., temperature, pressure, etc.). B. subtilis var. niger spore coupons were exposed to a range of temperatures from 125 C to 200 C in a vacuum oven (at <1 Torr). After the exposures, the spores were removed by sonication, dilutions were made, and the spores were plated using the pour plate method with tryptic soy agar. After 3 days incubation at 32 C, the number of colony-forming units was counted. Lethality rate constants and D-values were calculated at each temperature. The calculated D-values were: 27 minutes (at 125 C), 13 minutes (at 135 C), and <0.1 minutes (at 150 C). The 125 C and 135 C survivor curves appeared as concavedownward curves. The 150 C survivor curve appeared as a straight-line. Due to the prolonged ramp-up time to the exposure conditions, spore killing during the ramp-up resulted in insufficient data to draw curves for exposures at 160 C, 175 C, and 200 C. Exploratory experiments using novel techniques, with short ramp times, for performing high temperature exposures were also examined. Several of these techniques, such as vacuum furnaces, thermal spore exposure vessels, and laser heating of the coupons, will be discussed.

bacillus subtilis var niger↗

NASA NTRS2007

Pyrolysis of Large Black Liquor Droplets

This paper presents the results of experiments involving the pyrolysis of large black liquor droplets in the NASA KC-135 reduced gravity aircraft. The reduced gravity environment facilitated the study of droplets up to 9 mm in diameter extending the results of previous studies to droplet sizes that are similar to those encountered in recovery boilers. Single black liquor droplets were rapidly inserted into a 923 K oven. The primary independent variables were the initial droplet diameter (0.5 mm to 9 mm), the black liquor solids content (66.12% - 72.9% by mass), and the ambient oxygen mole fraction (0.0 - 0.21). Video records of the experiments provided size and shape of the droplets as a function of time. The results show that the particle diameter at the end of the drying stage (D(sub DRY) ) increases linearly with the initial particle diameter (D(sub O)). The results further show that the ratio of the maximum swollen diameter (D(sub MAX)) to D(sub O) decreases with increasing D(sub O) for droplets with D(sub O) less than 4 mm. This ratio was independent of D(sub O) for droplets with D(sub O) greater than 4 mm. The particle is most spherical at the end of drying, and least spherical at maximum swollen size, regardless of initial sphericity and droplet size.

Bartkus, Tadas P.↗

NASA NTRS2007

Gravity Probe B Timing System and Roll Phase Determination

An oven-controlled crystal oscillator at 16.368 MHz provides clock signals to all GP-B components and synchronizes the data collection, transmission and processing. The sampled science data signals are stamped with the vehicle time, a counter of the 10Hz data strobe divided down from the clock. The GPS receiver supplies an external reference for time transfer between the vehicle time and coordinated universal time. Ground and space flight tests show the time transfer error is within 1 microsecond. The time latency between the effective sample time of science signals and the stamped vehicle time is verified to 1 ms in the ground tests. The GP-B satellite is controlled to roll with a period of 77.5 sec about an axis along the direction to the guide star to average out the disturbance torques fixed to the body of the satellite and reduce the gyroscope readout noise. The roll phase is determined on the ground to high accuracy with the telemetry data from two star trackers and used in the data analysis to separate the drifts of gyroscope spin axes in the orbital plane and perpendicular to the orbital plane. The flight data shows that the roll phase is controlled to within 40 arcsec with a measurement uncertainty of 7 arcsec.

Jie, Li↗

NASA NTRS2007

Pyrolysis of Large Black Liquor Droplets

This paper presents the results of experiments involving the pyrolysis of large black liquor droplets in the NASA KC-135 reduced gravity aircraft. The reduced gravity environment facilitated the study of droplets up to 9 mm in diameter extending the results of previous studies to droplet sizes that are similar to those encountered in recovery boilers. Single black liquor droplets were rapidly inserted into a 923 K oven. The primary independent variables were the initial droplet diameter (0.5 mm to 9 mm), the black liquor solids content (66.12% - 72.9% by mass), and the ambient oxygen mole fraction (0.0 - 0.21). Video records of the experiments provided size and shape of the droplets as a function of time. The results show that the particle diameter at the end of the drying stage (D(sub DRY)) increases linearly with the initial particle diameter (D(sub O)). The results further show that the ratio of the maximum swollen diameter (D(sub MAX)) to D(sub O) decreases with increasing D(sub O) for droplets with D(sub O) less than 4 mm. This ratio was independent of D(sub O) for droplets with D(sub O) greater than 4 mm. The particle is most spherical at the end of drying, and least spherical at maximum swollen size, regardless of initial sphericity and droplet size.

Bartkus, Tadas P.↗

NASA NTRS2000

Uniform batch processing using microwaves

A microwave oven and microwave heating method generates microwaves within a cavity in a predetermined mode such that there is a known region of uniform microwave field. Samples placed in the region will then be heated in a relatively identical manner. Where perturbations induced by the samples are significant, samples are arranged in a symmetrical distribution so that the cumulative perturbation at each sample location is the same.

Barmatz, Martin B.↗