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The oxidative aging of 50-micron-thick films of LARC-TPI was studied using conventional thermogravimetric techniques and measurements of plane-stress fracture toughness. It was shown that at high temperature, most of the toughness loss occurred very early relative to the weight loss. The difficulties of interpreting TGA results in this regime and the problems of extrapolations to long times are discussed.
Eight urethane compounds were evaluated as possible replacement for the existing encapsulating compoounds for electrical cables for the Launch Support System at Kennedy Space Center (KSC). The existing encapsulating compound, PR-1535, contains the curative MOCA 4-4'-Methylene-BIS (2-chloroaniline), which is a suspect carcinogen and hence may be the subject of further restrictions of its use by the Occupational Safety and Health Administration (OSHA). The samples made in the configuration of cable joints and in the form of disks were evaluated for flammability and hypergolic compatibility. These also underwent accelerated weatherability tests that measured the residual hardness of the exposed samples. Three candidates and the existing compound passed the hardness test. Of these, only one candidate and the existing compound passed the flammability test. The thermal and hydrolytic stability (weatherability) of these samples was studied using thermogravimetric analysis (DSC) techniques. The TMA and DSC data correlated with the residual hardness data; whereas, the TGA data showed no correlation. A hypergolic compatibility test will be conducted on the compound V-356-HE80, which passed both the flammability and accelerated weatherability tests.
A chemical method of adding certain catalysts to improve the degradation process of a solid fuel is discussed. Thermogravimetric (TGA) analysis used to study the fundamental degradation behavior of a typical hybrid fuel (HTPB) shows that high surface temperatures increase the degradation rate. Fuels were tested in a laboratory-scale experimental hybrid rocket and their behavior was compared to a baseline behavior of HTPB fuel regression rates. It was found that a small amount of metal powder added to the fuel can significantly increase the regression rates.
The influence of the silver content and the oxygen partial pressure on the solidus temperature and the weight loss during melting of Bi2Sr2Ca1Cu2O(x) has been examined by means of DTA and TGA. By decreasing the oxygen partial pressure the solidus is lowered (e.g. del T = 59 C by decreasing pO2 from 1 atm to 0.001 atm) and the weight loss is increased. The addition of silver causes two effects: (1) the solidus is further decreased (e.g. 2 wt% Ag lower T (solidus) by up to 25 C, depending on the oxygen partial pressure); and (2) the weight loss during melting is reduced. Thick films (10-20 micron in thickness) with 0 and 5 wt% silver and bulk samples with) and 2.7 wt% silver were melt processed in flowing oxygen on a silver substrate in the DTA, allowing the observation of the melting process and a good temperature control. The critical current densities are vigorously dependent on the maximum processing temperature. The highest j(sub c) in thick films (8000 A/sq cm at 77 K, O T) was reached by melting 7 C above the solidus temperature. The silver addition shows no significant effect on the processing parameters or the superconducting properties. The highest j(sub c) for bulk samples (1 mm in thickness) was obtained by partial melting at 900 C or 880 C, depending on the silver content of the powder (0 or 2.7 wt%). The j(sub c) of the samples is slightly enhanced from 1800 A/sq cm (at 77 K, O T) to 2000 A/sq cm by the silver addition. To be able to reach at least 80% of the maximum critical current density, the temperature has to be controlled in a window of 5 C for thick films and 17 C for bulk samples.
Semi-interpenetrating (S-IPN) network polyimids were made from different proportions of LaRC RP46 (a thermosetpolyimid) and LaRC BDTA-ODA (a thermoplastic polyimid). The ultimate goal of this networking is to improve the mechanical properties of the thermoset polyimid. Positron lifetime study was made to calculate lifetime based on second component of the life time spectra and the free volume & microvoid size. All these properties tend to decrease steadily with increasing thermoset content except at the 50 percent thermoset level where these properties show sudden drop. This result contradicts with the initial expectation that the blend properties should change gradually if it were a solid solution of thermoset (TSP) and thermoplastic (TPP) components. Thermal analyses (TMA, DSC, DMA & TGA) were run to complement the positron life time studies. The TMA and DSC studies confirm the contradiction mentioned above. Further experimentation with S-IPN polymers made at TSP/TTP content around 50/50 level are being conducted to explain this anomaly. Scanning electron microscope study of the S-IPN polyimid samples is under way in order to detect morphological differences which might help explain the phenomenon mentioned above.
The oxidation behavior of reaction-formed silicon carbide (RFSC) ceramics was investigated in the temperature range of 1100 to 1400 C. The oxidation weight change was recorded by TGA; the oxidized materials were examined by light and electron microscopy, and the oxidation product by x-ray diffraction analysis (XRD). The materials exhibited initial weight loss, followed by passive weight gain (with enhanced parabolic rates, k(sub p)), and ending with a negative (logarithmic) deviation from the parabolic law. The weight loss arose from the oxidation of residual carbon, and the enhanced k(sub p) values from internal oxidation and the oxidation of residual silicon, while the logarithmic kinetics is thought to have resulted from crystallization of the oxide. The presence of a small amount of MoSi, in the RFSC material caused a further increase in the oxidation rate. The only solid oxidation product for all temperatures studied was silica.
Pure coupons of chemically vapor deposited (CVD) SiC were oxidized for 100 h in dry flowing oxygen at 1300 C. The oxidation kinetics were monitored using thermogravimetry (TGA). The experiments were first performed using high-purity alumina reaction tubes. The experiments were then repeated using fused quartz reaction tubes. Differences in oxidation kinetics, scale composition, and scale morphology were observed. These differences were attributed to impurities in the alumina tubes. Investigators interested in high-temperature oxidation of silica formers should be aware that high-purity alumina can have significant effects on experiment results.
One of today's most important and challenging technological problems is the development of advanced materials and processes required to design and build a fleet of supersonic High Speed Civil Transport (HSCT) airliners, a follow-up to the Concorde SST. The innovative combustor designs required for HSCT engines will need high-temperature materials with long-term environmental stability. Higher combustor liner temperatures than today's engines and the need for lightweight materials will require the use of advanced ceramic-matrix composites (CMC's) in hot-section components. The HSCT is just one example being used to demonstrate the need for such materials. This thesis evaluates silicon carbide (SiC) as a potential base material for HSCT and other similar applications. Key issues are the environmental durability for the materials of interest. One of the leading combustor design schemes leads to an environment which will contain both oxidizing and reducing gas mixtures. The concern is that these environments may affect the stability of the silica (SiO2) scale on which SiC depends for environmental protection. A unique High Pressure Burner Rig (HPBR) was developed to simulate the combustor conditions of future gas turbine engines, and a series of tests were conducted on commercially available SiC material. These tests are intended as a feasibility study for the use of these materials in applications such as the HSCT. Linear weight loss and surface recession of the SiC is observed as a result of SiO2 volatility for both fuel-lean and fuel-rich gas mixtures. These observations are compared and agree well with thermogravimetric analysis (TGA) experiments. A strong Arrhenius-type temperature dependence exists. In addition, the secondary dependencies of pressure and gas velocity are defined. As a result, a model is developed to enable extrapolation to points outside the experimental space of the burner rig, and in particular, to potential gas turbine engine conditions.
The oxidation kinetics of CVD SiC were monitored by thermogravimetric analysis (TGA) in a 50% H2O/50% O2 gas mixture flowing at 4.4 cm/s for temperatures between 1200 and 1400 C. Paralinear weight change kinetics were observed as the water vapor oxidized the SiC and simultaneously volatilized the silica scale. The long-term degradation rate of SiC is determined by the volatility of the silica scale. Rapid SiC surface recession rates were estimated from these data for actual aircraft engine combustor conditions.
Due to the difficulty in processing polyimides with high temperature stability and good solvent resistance, we have synthesized high performance polyimides with bicyclo(2.2.2)-oct-7-ene ring system which can easily be fabricated into films and fibers and subsequently converted to the more stable aromatic polyimides. In order to improve processability, we prepared two polyimides by reacting 1,4-phenylenediamine and 1,3phenylediamine with bicyclo(2.2.2)-7-octene-2,3,5,6-tetracarboxylic dianhydride. The polyimides were characterized by FTIR, FTNMR, solubility and thermal analysis. Thermogravimetric analysis (TGA) showed that the 1,4-phenylenediamine and 1,3-phenylenediamine containing polyimides were stable up to 460 and 379 C, respectively under nitrogen atmosphere. No melting transitions were observed for both polyimides. The 1,4-phenylenediamine containing polyimide is partially soluble in dimethyl sulfoxide, methane sulfonic acid and soluble in sulfuric acid at room temperature. The 1,3-phenylenediamine containing polyimide is partially soluble in dimethyl sulfoxide, tetramethyl urea, N,N-dimethyl acetamide and soluble in methane sulfonic acid and sulfuric acid.
Thermal decomposition activation energies have been determined using two methods of Thermogravimetric Analysis (TGA), with good correlation being obtained between the two techniques. Initial heating curves indicated a two-component system for Coflon (i.e. polymer plus placticizer) but a single component system for Tefzel. Two widely differing activation energies were for Coflon supported this view, 15 kcl/mol being associated with plasticizer, and 40 kcal/mol with polymer degradation. With Tefzel, values were 40-45 kcal/mol, the former perhaps being associated with a low molecular weight fraction. Appropriate acceleration factors have been determined. Thermomechanical Analysis (TMA) has shown considerable dimensional change during temperature cycles. For unaged pipe sections heating to 100 C and then holding the temperature resulted in a stable thickness increase of 2%, whereas the Coflon thickness decreased continuously, reaching -4% in 2.7 weeks. Previously strained tensile bars of Tefzel expanded on cooling during TMA. SEM performed on H2S-aged Coflon samples showed significant changes in both physical and chemical nature. The first may have resulted from explosive decompression after part of the aging process. Chemically extensive dehydrofluorination was indicated, and sulfur was present as a result of the aging. These observations indicate that chemical attack of PVDF can occur in some circumstances.
The objectives of this research program were to reduce the manufacturing costs of variable stator vane bushings by 1) eliminating the expensive carbon fiber braiding operation, 2) replacing the batch mode impregnation, B-stage, and cutting operations with a continuous process, and 3) reducing the molding cycle and machining operations with injection molding to achieve near-net shapes. Braided bushings were successfully fabricated with both AMB-17XLD and AMB-TPD resin systems. The composite bushings achieved high glass transition temperature after post-cure (+300 C) and comparable weight loss to the PNM-15 bushings. ANM-17XLD bushings made with "batch-mode" molding compound (at 0.5 in. fiber length) achieved a +300 lb-force flange break strength which was superior to the continuous braided-fiber reinforced bushing. The non-MDA resin technology developed in this contract appears attractive for bushing applications that do not exceed a 300 C use temperature. Two thermoplastic polyimide resins were synthesized in order to generate injection molding compound powders. Excellent processing results were obtained at injection temperatures in excess of 300 C. Micro-tensile specimens were produced from each resin type and the Tg measurements (by TMA) for these samples were equivalent to AURUM(R). Thermal Gravimetric Analysis (TGA) conducted at 10 C/min showed that the non-MDA AMB-type polyimide thermoplastics had comparable weight loss to PMR-15 up to 500 C.
Chemically-vapor-deposited silicon carbide (CVD SiC) was oxidized in carbon dioxide (CO2) at temperatures of 1200-1400 C for times between 100 and 500 hours at several gas flow rates. Oxidation weight gains were monitored by thermogravimetric analysis (TGA) and were found to be very small and independent of temperature. Possible rate limiting kinetic laws are discussed. Oxidation of SiC by CO2 is negligible compared to the rates measured for other oxidants typically found in combustion environments: oxygen and water vapor.
The durability of polymer matrix composites exposed to harsh environments is a major concern. Surface degradation and damage are observed in polyimide composites used in air at 125-300 C. It is believed that diffusion of oxygen into the material and oxidative chemical reactions are responsible. Previous work has characterized and modeled diffusion behavior, and thermogravimetric analyses (TGAS) have been carried out in nitrogen, air, and oxygen to provide quantitative information on thermal and oxidative reactions. However, the model developed using these data did not successfully extrapolate TGA data down to conditions seen in service. A test program that focuses on lower temperatures and makes use of isothermal tests was undertaken to achieve a better understanding of the degradation reactions under use conditions. A new, low-cost technique was developed to collect chemical degradation data for isothermal tests lasting over 200 hours in the temperature range 125-300 C. Results indicate complex behavior not captured by the previous model, including the presence of weight-adding reactions. Weight gain reactions dominated in the 125-225 C temperature range, while weight loss reactions dominated beyond 225 C. The data obtained from isothermal tests and earlier TGAs is used to develop an advanced model of the material behavior.
Blackglas(Trademark) polysiloxane systems produce silicon oxycarbide glasses by pyrolysis in inert atmosphere. The silicon oxycarbides evidence oxidative degradation that limits their lifetime as composite matrices. The present study characterizes bonding rearrangements in the oxycarbide network accompanying increases in pyrolysis temperature. It also addresses the changes in susceptibility to oxidation due to variations in the distribution of Si bonded species obtained under different processing conditions. The study is carried out using Si-29 nuclear magnetic resonance (NMR) spectroscopy and a design of experiments approach to model the oxidation behavior. The NMR results are compared with those obtained by thermogravimetric analysis (TGA). Samples pyrolyzed under inert conditions are compared to those pyrolyzed in reactive ammonia environments.
Chemically-vapor-deposited silicon carbide (CVD SiC) was oxidized in carbon dioxide (CO2) at temperatures of 1200-1400 C for times between 96 and 500 h at several gas flow rates. Oxidation weight gains were monitored by thermogravimetric analysis (TGA) and were found to be very small and independent of temperature. Possible rate limiting kinetic mechanisms are discussed. Passive oxidation of SiC by CO2 is negligible compared to the rates measured for other oxidants that are also found in combustion environments, oxygen and water vapor.
Several instruments including the Cahn Microbalance the Knudsen Cell, the micro-CVCM, and the vacuum Thermogravimetric Analyzer (TGA) were used in the testing of a graphite epoxy (GR/EP) composite that is proposed for use as a rigidizing element of an inflatable deployment system. This GR/EP will be cured in situ. The purpose of this testing is to estimate the gaseous production resulting from the curing of the GR/EP composite, to predict the resulting pressure, and to calculate the required venting. Every test was conducted under vacuum at 125 C for 24 hours. Upon comparison of the results, the ASTM E-595 was noted to have given readings that were consistently lower than those obtained using the other instruments, which otherwise provided similar results. The GR/EP was tested using several different geometric arrangements. This paper describes the analysis evaluating the molecular and continuum flow of the outgassing products issuing from the exit port of the ASTM E-595 system. The effective flow conductance provided by the physical dimensions of the vent passage of the ASTM E-595 system and that of the material sample among other factors were investigated to explain the reduced amount of outgassing released during the 24-hour test period
A mechanically undensified aromatic polyimide foam is made from an aromatic polyimide precursor solid residuum and has the following combination of properties: a density according to ASTM D-3574A of about 0.5 pounds/cu.ft to about 20 pounds/cu.ft; a compression strength according to ASTM D-3574C of about 1.5 psi to about 1500 psi; and a limiting oxygen index according to ASTM D-2863 of about 35% oxygen to about 75% oxygen at atmospheric pressure. The aromatic polyimide foam has no appreciable solid inorganic contaminants which are residues of inorganic blowing agents. The aromatic polyimide which constitutes the aromatic polyimide foam has a glass transition temperature (Tg) by differential scanning calorimetry of about 235 C to about 400 C; and a thermal stability of 0 to about 1% weight loss at 204 C as determined by thermogravinietric analysis (TGA). The aromatic polyimide foam has utility as foam insulation and as structural foam, for example, for aeronautical, aerospace and maritime applications.