Search NASA⌕ Search

SEARCH · Search NASA

Results for “Thermogravimetric analysis”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 163 records · Page 9
All sourcesNASA NTRSDOE OSTI
NASA NTRS1994

Light Weight Ceramic Ablators for Mars Follow-on Mission Vehicle Thermal Protection System

New Light Weight Ceramic Ablators (LCA) were produced by using ceramic and carbon fibrous substrates, impregnated with silicone and phenolic resins. The special infiltration techniques (patent pending) were developed to control the amount of organic resins in the highly porous fiber matrices so that the final densities of LCA's range from 0.22 to 0.24 g/cc. This paper presents the thermal and ablative performance of the Silicone Impregnated Reusable Ceramic Ablators (SIRCA) in simulated entry conditions for Mars-Pathfinder in the Ames 60 MW Interaction Heating Facility (I HF). Arc jet test results yielded no evidence of char erosion and mass loss at high stagnation pressures to 0.25 atm. Minimal silica melt was detected on surface char at a stagnation pressure of 0.31 atm. Four ceramic substrates were used in the production of SIRCA's to obtain the effective of boron oxide present in substrate so the thermal performance of SIRCA's. A sample of SIRCA was also exposed to the same heating condition for five cycles and no significant mass loss or recession was observed. Tensile testing established that the SIRCA tensile strength is about a factor of two higher than that of the virgin substrates. Thermogravimetric Analysis (TGA) of the char in nitrogen and air showed no evidence of free carbon in the char. Scanning Electron Microscopy of the post test sample showed that the char surface consists of a fibrous structure that was sealed with a thin layer of silicon oxide melt.

Tran, Huy K.↗
NASA NTRS2001

The Tribological Properties of Several Silahydrocarbons for Use in Space Mechanisms

Silahydrocarbons are members of a relatively new class of liquid lubricants with great potential for use in space mechanisms. They are unimolecular species consisting of silicon, carbon, and hydrogen. They possess unique wear, viscosity, and volatility properties while retaining the ability to solubilize conventional additives. The tribological properties of several members of this class, including tri, tetra- and penta-compounds, are presented. These properties include: viscosity-temperature (ASTM D446), viscosity-pressure coefficient, vapor pressure, volatility, lubricant lifetimes, traction, reciprocating and four ball wear rates and bearing performance. Lubricant lifetimes were determined using a vacuum ball bearing simulator, the spiral orbit tribometer (SOT). Wear was measured using a Cameron Plint reciprocating tribometer and wear rates with a vacuum four ball tribometer. Conventional viscometry was used for viscosity-temperature measurements and a Knudsen cell for vapor pressure. Vacuum Thermogravimetric Analysis (TGA) was also used for volatility measurements. Pressure viscosity coefficients (a values) were estimated from EHL (elastohydrodynamic lubrication) film thickness measurements. Traction coefficients were measured with a twin disk traction rig. Bearing tests were performed in a vacuum bearing test facility. These properties are compared to existing state-of-the-art space lubricants.

Jones, W. R., Jr.↗
NASA NTRS2002

Preparation and Characterization of Polyimide/Organoclay Nanocomposites

Organically modified montmorrrillonite clay, containing a long chain aliphatic quarternary ammonium cation, was used to prepare polyimide/organoclay hybrids. Several approaches were examined in an attempt to achieve fully exfoliated nanocomposites. These included simple mixing of the clay in a pre-made high molecular weight poly(amide acid) solution; simple mixing followed by sonication of the organoclay/poly(amide acid) solutions; and the preparation of high molecular weight poly(amide acid)s in the presence of the organoclay dispersed in N-methyl-2-pyrrolidinone (NMP). The best results were obtained using the in-situ polymerization approach. The resulting nanocomposite films (both amide acid and imide), containing 3-8% by weight of organoclay, were characterized by differential scanning calorimetry (DSC), dynamic thermogravimetric analysis (TGA), transmission electron microscopy (TEM), X-ray diffraction (XRD), and thin film tensile properties. A significant degree of dispersion was observed in the nanocomposite films of the amide acid and the imide. After thermal treatment of amide acid films to effect imidization, in both air and nitrogen, the films were visually darker than control films without clay and the level of clay dispersion appeared to have decreased. In the latter case, the separation between the layers of the clay decreased to a spacing less than that present in the original organoclay. These observations suggest that thermal degradation of the aliphatic quarternary ammonium cation occurred likely during thermal treatment to effect imidization and solvent removal. These thermal degradation effects were less pronounced when thermal treatment was performed under nitrogen. The polyimide/organoclay hybrid films exhibited higher room temperature tensile moduli and lower strength and elongation to break than the control films.

Delozier, D. M.↗
NASA NTRS2002

Effect of Environment on Stress-Rupture Behavior of a Carbon Fiber-Reinforced Silicon Carbide (C/SiC) Ceramic Matrix Composite

Stress-rupture tests were conducted in air, vacuum, and steam-containing environments to identify the failure modes and degradation mechanisms of a carbon fiber-reinforced silicon carbide (C/SiC) composite at two temperatures, 600 and 1200 C. Stress-rupture lives in air and steam containing environments (50 - 80% steam with argon) are similar for a composite stress of 69 MPa at 1200 C. Lives of specimens tested in a 20% steam/argon environment were about twice as long. For tests conducted at 600 C, composite life in 20% steam/argon was 20 times longer than life in air. Thermogravimetric analysis of the carbon fibers was conducted under similar conditions to the stress-rupture tests. The oxidation rate of the fibers in the various environments correlated with the composite stress-rupture lives. Examination of the failed specimens indicated that oxidation of the carbon fibers was the primary damage mode for specimens tested in air and steam environments at both temperatures.

Verrilli, Michael J.↗
NASA NTRS2003

Sol-Gel Precursors for Ceramics from Minerals Simulating Soils from the Moon and Mars

Recent NASA mission plans for the human exploration of our Solar System has set new priorities for research and development of technologies necessary to enable a long-term human presence on the Moon and Mars. The recovery and processing of metals and oxides from mineral sources on other planets is under study to enable use of ceramics, glasses and metals by explorer outposts. We report some preliminary results on the production of sol-gel precursors for ceramic products using mineral resources available in Martian or Lunar soil. The presence of SiO2, TiO2, and A12O3 in both Martian (44 wt.% SiO2, 1 wt.% TiO2, 7 wt.% Al2O3) and Lunar (48 wt.% SiO2, 1.5 wt.% TiO2, 16 wt.% Al2O3) soils and the recent developments in chemical processes to solubilize silicates using organic reagents and relatively little energy indicate that such an endeavor is possible. In order to eliminate the risks involved in the use of hydrofluoric acid to dissolve silicates, two distinct chemical routes are investigated to obtain soluble silicon oxide precursors from Lunar and Martian simulant soils. Clear sol-gel precursors have been obtained by dissolution of silica from Lunar simulant soil in basic ethylene glycol (C2H4(OH)2) solutions to form silicon glycolates. Thermogravimetric Analysis and X-ray Photoelectron Spectroscopy were used to characterize the elemental composition and structure of the precursor molecules. Further concentration and hydrolysis of the products was performed to obtain gel materials for evaluation as ceramic precursors. In the second set of experiments, we used the same starting materials to synthesize silicate esters in acidified alcohol mixtures. Preliminary results indicate the presence of silicon alkoxides in the product of distillation.

Sibille, Laurent↗
NASA NTRS2003

Preparation and Characterization of Space Durable Polymer Nanocomposite Films from Functionalized Carbon Nanotubes

Low color, flexible, space durable polyimide films with inherent, robust electrical conductivity have been under investigation as part of a continuing materials development activity for future NASA space missions involving Gossamer structures. Electrical conductivity is needed in these films to dissipate electrostatic charge build-up that occurs due to the orbital environment. One method of imparting conductivity is through the use of single walled carbon nanotubes (SWNTs). However, the incompatibility and insolubility of the SWNTs severely hampers their dispersion in polymeric matrices. In an attempt to improve their dispersability, SWNTs were functionalized by the reaction with an alkyl hydrazone. After this functionalization, the SWNTs were soluble in select solvents and dispersed more readily in the polymer matrix. The functionalized SWNTs were characterized by Raman spectroscopy and thermogravimetric analysis (TGA). The functionalized nanotubes were dispersed in the bulk of the films using a solution technique. The functionalized nanotubes were also applied to the surface of polyimide films using a spray coating technique. The resultant polyimide nanocomposite films were evaluated for nanotube dispersion, electrical conductivity, mechanical, and optical properties and compared with previously prepared polyimide-SWNT samples to assess the effects of SWNT functionalization.

Delozier, D. M.↗
NASA NTRS2003

Attachment of Single-wall Carbon Nanotubes (SWNTs) on Platinum Surfaces by Self-Assembling Techniques

Single-wall carbon nanotubes (SWNTs) are very interesting materials because of their morphology, electronic and mechanical properties. Its morphology (high length-to-diameter ratio) and electronic properties suggest potential application of SWNTs as anode material for lithium ion secondary batteries. The introduction of SWNTs on these types of sources systems will improve their performance, efficiency, and capacity to store energy. A purification method has been applied for the removal of iron and amorphous carbon from the nanotubes. Unpurified and purified SWNTs were characterized by transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). In order to attach carbon nanotubes on platinum electrode surfaces, a self-assembled monolayer (SAM) of 4-aminothiophenol (4-ATP) was deposited over the electrodes. The amino-terminated SAM obtained was characterized by cyclic voltammetry, X-ray photoelectron spectroscopy (XPS), and Fourier-transforms infrared (FTIR) spectroscopy. Carbon nanotubes were deposited over the amino-terminated SAM by an amide bond formed between SAM amino groups and carboxylic acid groups at the open ends of the carbon nanotubes.This deposition was characterized using Raman spectroscopy and Scanning Electron microscopy (SEM).

Rosario-Castro, Belinda I.↗
NASA NTRS2004

Flame Retardant Epoxy Resins

As part of a program to develop fire resistant exterior composite structures for future subsonic commercial aircraft, flame retardant epoxy resins are under investigation. Epoxies and their curing agents (aromatic diamines) containing phosphorus were synthesized and used to prepare epoxy formulations. Phosphorus was incorporated within the backbone of the epoxy resin and not used as an additive. The resulting cured epoxies were characterized by thermogravimetric analysis, propane torch test, elemental analysis and microscale combustion calorimetry. Several formulations showed excellent flame retardation with phosphorous contents as low as 1.5% by weight. The fracture toughness of plaques of several cured formulations was determined on single-edge notched bend specimens. The chemistry and properties of these new epoxy formulations are discussed.

Thompson, C. M.↗
NASA NTRS2000

Space Environmentally Stable Polyimides and Copolyimides

Polyimides with a unique combination of properties including low color in thin films, atomic oxygen (AO), ultra-violet (UV) radiation resistance, solubility in organic solvents in the imide form, high glass transition (T(sub g)) temperatures and high thermal stability have been prepared and characterized. The polymers were prepared by reacting a novel aromatic diamine with aromatic dianhydrides in a polar aprotic solvent. The solubility of the polymers in the imide form as well as the color density of thin films were dependent upon the chemical structure of the dianhydride. Several thin films (25-50 mm thick) prepared by solution casting of amide acid or imide solutions exhibited very low color and high optical transparency (approximately 90%) as determined by UV/visible spectroscopy. The polymers exhibited T(sub g)s >200 C depending upon the structure of the dianhydride and temperatures of 5% weight loss approximately 500C in air as determined by dynamic thermogravimetric analysis. Thin films coated with silver/inconel were exposed to a high fluence of AO and 1000 equivalent solar hours of UV radiation. The effects of these exposures on optical properties were minor. These space environmentally durable polymers are potentially useful in a variety of applications on spacecraft such as thin film membranes on antennas, second-surface mirrors, thermal/optical coatings and multi-layer thermal insulation (MLI) blanket materials. The chemistry, physical and mechanical properties of the polymers as well as their responses to AO and UV exposure will be discussed.

Watson, Kent A.↗
NASA NTRS2003

Oxidation Kinetics and Strength Degradation of Carbon Fibers in a Cracked Ceramic Matrix Composite

Experimental results and oxidation modeling will be presented to discuss carbon fiber susceptibility to oxidation, the oxidation kinetics regimes and composite strength degradation and failure due to oxidation. Thermogravimetric Analysis (TGA) was used to study the oxidation rates of carbon fiber and of a pyro-carbon interphase. The analysis was used to separately obtain activation energies for the carbon constituents within a C/SiC composite. TGA was also conducted on C/SiC composite material to study carbon oxidation and crack closure as a function of temperature. In order to more closely match applications conditions C/SiC tensile coupons were also tested under stressed oxidation conditions. The stressed oxidation tests show that C/SiC is much more susceptible to oxidation when the material is under an applied load where the cracks are open and allow for oxygen ingress. The results help correlate carbon oxidation with composite strength reduction and failure.

Halbig, Michael C.↗
NASA NTRS2004

Robust Joining Technology for Solid Oxide Fuel Cells Applications

Recently there has been a great deal of interest in research development and commercialization of solid oxide fuel cells (SOFCs). Joining and sealing are critical issues that will need to be addressed before SOFCs can truly perform as expected. Ceramics and metals can be difficult to join together, especially when the joint must withstand up to 900 C operating temperature of the SOFCs. The goal of the present study is to find the most suitable braze material for joining of yttria stabilized zirconia (YSZ) to stainless steel. A number of commercially available braze materials TiCuSil, TiCuNi, Copper-ABA, Gold-ABA and Gold-ABA-V have been evaluated. The oxidation behavior of the braze materials and steel substrates in air was also examined through thermogravimetric analysis. The microstructure and composition of the brazed regions have been examined by optical and scanning electron microscopy and eDS analysis. Effect of braze composition and processing conditions on the interfacial microstructure and composition of the joint regions will be presented.

Shpargel, Tarah P.↗
NASA NTRS2004

Growth of Multi-Walled Carbon Nanotubes by Injection CVD Using Cyclopentadienyliron Dicarbonyl Dimer and Cyclooctatetraene Iron Tricarbonyl

Preferential oriented multiwalled carbon nanotubes were prepared by the injection chemical vapor deposition (CVD) method using either cyclopentadienyliron dicarbonyl dimer or cycloctatetraene iron tricarbonyl as the iron catalyst source. The catalyst precursors were dissolved in toluene as the carrier solvent for the injections. The concentration of the catalyst was found to influence both the growth of the nanotubes as well as the amount of iron in the deposited material. As deposited the multiwalled carbon nanotubes contained as little as 2.8% iron by weight. The material was deposited onto tantalum foil and fused silica substrates. The nanotubes were characterized by scanning electron microscopy, transmission electron microscopy, Raman spectroscopy and thermogravimetric analysis. This synthetic route provides a simple and scalable method to deposit MWNTs with a low defect density, low metal content and preferred orientation.

Harris, Jerry D.↗
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

Synthesis, Characterization and Decomposition Studies of Tris(N,N-dibenzyldithiocarbamato) Indium(III): Chemical Spray Deposition of Polycrystalline CuInS2 on Copper Films

Tris(bis(phenylmethyl)carbamodithioato-S,S ), commonly referred to as tris(N,Ndibenzyldithiocarbamato) indium(III), In(S2CNBz2)3, was synthesized and characterized by single crystal X-ray crystallography. The compound crystallizes in the triclinic space group P1 bar with two molecules per unit cell. The material was further characterized using a novel analytical system employing the combined powers of thermogravimetric analysis, gas chromatography/mass spectrometry and Fourier-Transform infrared spectroscopy to investigate its potential use as a precursor for the chemical vapor deposition (CVD) of thin film materials for photovoltaic applications. Upon heating, the material thermally decomposes to release CS2 and benzyl moieties in to the gas phase, resulting in bulk In2S3. Preliminary spray CVD experiments indicate that In(S2CNBz2)3 decomposed on a Cu substrate reacts to produce stoichiometric CuInS2 films.

Hehemann, David G.↗
NASA NTRS2004

Oxidation of High-temperature Alloy Wires in Dry Oxygen and Water Vapor

Small diameter wires (150 to 250 microns) of the high temperature alloys Haynes 188, Haynes 230, Haynes 230, Haynes 214, Kanthal Al and PM2000 were oxidized at 1204 C in dry oxygen or 50% H2O /50% O2 for 70 Hours. The oxidation kinetics were monitored using a thermogravimetric technique. Oxide phase composition and morphology of the oxidized wires were determined by X-ray diffraction,field emission scanning electron microscopy, and energy dispersive spectroscopy. The alumina-forming alloys, Kanthal Al and PM2000, out-performed the chromia-forming alloys under this conditions. PM2000 was recommended as the most promising candidate for advanced hybrid seal applications for space reentry control surface seals or hypersonic propulsion system seals. This study also demonstrated that thermogravimetric analysis of small diameter wires is a powerful technique for the study of oxide volatility, oxide adherence, and breakaway oxidation.

Opila, Elizabeth J.↗
NASA NTRS1997

Volatile Reaction Products From Silicon-Based Ceramics in Combustion Environments Identified

Silicon-based ceramics and composites are prime candidates for use as components in the hot sections of advanced aircraft engines. These materials must have long-term durability in the combustion environment. Because water vapor is always present as a major product of combustion in the engine environment, its effect on the durability of silicon-based ceramics must be understood. In combustion environments, silicon-based ceramics react with water vapor to form a surface silica (SiO2) scale. This SiO2 scale, in turn, has been found to react with water vapor to form volatile hydroxides. Studies to date have focused on how water vapor reacts with high-purity silicon carbide (SiC) and SiO2 in model combustion environments. Because the combustion environment in advanced aircraft engines is expected to contain about 10-percent water vapor at 10-atm total pressure, the durability of SiC and SiO2 in gas mixtures containing 0.1- to 1-atm water vapor is of interest. The reactions of SiC and SiO2 with water vapor were monitored by measuring weight changes of sample coupons in a 0.5-atm water vapor/0.5-atm oxygen gas mixture with thermogravimetric analysis.

Opila, Elizabeth J.↗
NASA NTRS2001

Long-Term Durability of a Matrix for High-Temperature Composites Predicted

Polymer matrix composites (PMC's) are being increasingly used in applications where they are exposed for long durations to harsh environments such as elevated temperatures, moisture, oils and solvents, and thermal cycling. The exposure to these environments leads to the degradation of structures made from these materials. This also affects the useful lifetimes of these structures. Some of the more prominent aerospace applications of polymer matrix composites include engine supports and cowlings, reusable launch vehicle parts, radomes, thrust-vectoring flaps, and the thermal insulation of rocket motors. This demand has led to efforts to develop lightweight, high-strength, high-modulus materials that have upper-use temperatures over 316 C. A cooperative program involving two grants to the Massachusetts Institute of Technology and in-house work at the NASA Glenn Research Center was conducted to identify the mechanisms and the measurement of mechanical and physical properties that are necessary to formulate a mechanism-based model for predicting the lifetime of high-temperature polymer matrix composites. The polymer that was studied was PMR-15 polyimide, a leading matrix resin for use in high-temperature-resistant aerospace composite structures such as propulsion systems. The temperature range that was studied was from 125 to 316 C. The diffusion behavior of PMR-15 neat resin was characterized and modeled. Thermogravimetric analysis (TGA) was also conducted in nitrogen, oxygen, and air to provide quantitative information on thermal and oxidative degradation reactions. A new low-cost technique was developed to collect chemical degradation data for isothermal tests lasting up to 4000 hr in duration. In the temperature range studied, results indicate complex behavior that was not observed by previous TGA tests, including the presence of weight-gain reactions. These were found to be significant in the initial periods of aging from 125 to 225 C. Two types of weight loss reactions dominated at aging temperatures above 225 C. One was concentrated at the surface of the polymer and was very active at temperatures above 225 C. The second was observed to dominate in the latter stages of aging at temperatures below 260 C. This three-reaction model satisfactorily explains past findings that the degradation mechanism of PMR-15 appears to change around 316 C. It also indicates that the second weight gain mechanism is a significant factor at temperatures below 204 C. On the basis of these results, a predictive model was developed for the thermal degradation of PMR-15 at 316 C. A comparison of data generated by this model with actual experimental data is shown in the following figure.

Bowles, Kenneth J.↗
NASA NTRS2002

Effect of Environment on the Stress- Rupture Behavior of a C/SiC Composite Studied

Advanced reusable launch vehicles will likely incorporate fiber-reinforced ceramic matrix composites (CMC's) in critical propulsion and airframe components. The use of CMC's is highly desirable to save weight, improve reuse capability, and increase performance. One of the candidate CMC materials is carbon-fiber-reinforced silicon carbide (C/SiC). In potential propulsion applications, such as turbopump rotors and nozzle exit ramps, C/SiC components will be subjected to a service cycle that includes mechanical loading under complex, high-pressure environments containing hydrogen, oxygen, and steam. Degradation of both the C fibers and the SiC matrix are possible in these environments. The objective of this effort was to evaluate the mechanical behavior of C/SiC in various environments relevant to reusable launch vehicle applications. Stress-rupture testing was conducted at the NASA Glenn Research Center on C/SiC specimens in air and steam-containing environments. Also, the oxidation kinetics of the carbon fibers that reinforce the composite were monitored by thermogravimetric analysis in the same environments and temperatures used for the stress-rupture tests of the C/SiC composite specimens. The stress-rupture lives obtained for C/SiC tested in air and in steam/argon mixtures are shown in the following bar chart. As is typical for most materials, lives obtained at the lower temperature (600 C) are longer than for the higher temperature (1200 C). The effect of environment was most pronounced at the lower temperature, where the average test duration in steam at 600 C was at least 30 times longer than the lives obtained in air. The 1200 C data revealed little difference between the lives of specimens tested in air and steam at atmospheric pressure.

Verrilli, Michael J.↗