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Polymers were tested and allowed to outgas isothermally at 125 C and .000001 torr or less. The performance was investigated by thermogravimetric analysis from room temperature to 450 C or until the substance decomposed.
Analogues of methylene dianilines were synthesized, in which the methylene group between the two aromatic nuclei was replaced by various perfluoroalkylene linkage. The hydrolytic thermal, and thermal oxidative stabilities of PMR Polyimides derived from these diamines were determined. Three types of PMR Polyimide discs were fabricated from the dimethyl ester of 3,3', 4,4'-benzophenonetetracarboxylic acid, the methyl ester of 5-norbornene-2,3-dicarboxylic acid, and one of the following three diamines: methyl dianiline, 1,3-bis(4-aminophenyl)hexafluoropropane, and 2,2-bis(4-aminophenyl)hexafluoropropane. The polyimide based on 2,2-bis(4-aminophenyl)hexafluoropropane exhibited the best hydrolytic, thermal, and thermal oxidative stability as determined by moisture uptake and thermogravimetric analysis.
The thermochemical and flammability characteristics of some typical thermoplastic materials currently in use and others being considered for use in aircraft interiors are described. The properties studied included (1) thermal mechanical properties such as glass transition and melt temperature, (2) changes in polymer enthalpy by differential scanning calorimetry, (3) thermogravimetric analysis in an anaerobic and oxidative environment, (4) oxygen index, (5) smoke evolution, (6) relative toxicity of the volatile products of pyrolysis, and (7) selected physical properties. The generic polymers which were evaluated included: acrylonitrile-butadiene-styrene, bisphenol A polycarbonate, bisphenol fluorenone carbonatedimethylsiloxane block polymer, phenolphthalein-bisphenol A polycarbonate, phenolphthalein polycarbonate, polyether sulfone, polyphenylene oxide, polyphenylene sulfide, polyaryl sulfone, chlorinated polyvinyl chloride homopolymer, polyvinyl fluoride, and polyvinylidene fluoride. Processing parameters including molding characteristics of some of the advanced polymers are described. Test results and relative rankings of some of the flammability, smoke and toxicity properties are presented.
The thermochemical and flammability properties of some thermally stable polymers considered for use in aircraft interiors are described. The properties studied include: (1) thermomechanical properties such as glass transition and melt temperature; (2) dynamic thermogravimetric analysis in anaerobic environment; (3) flammability properties such as oxygen index, flame spread, and smoke evolution; and (4) selected physical properties. The thermoplastic polymers evaluated included polyphenylene sulfide, polyaryl sulfone, 9,9-bis(4-hydroxyphenyl)-fluorene polycarbonate-poly(dimethylsiloxane) and polyether sulfone. The thermoset polymers evaluated included epoxy, bismaleimide, a modified phenolic and polyaromatic melamine resin. These resins were primarily used in the fabrication of glass reinforced prepregs for the construction of experimental panels. Test results and relative rankings of some of the flammability parameters are presented and the relationship of the molecular structure, char yield, and flammability properties of these polymers are discussed.
The thermochemical and flammability properties of some thermally stable polymers considered for use in aircraft interiors are described. The properties studied include: (1) thermomechanical properties such as glass transition and melt temperature; (2) dynamic thermogravimetric analysis in anaerobic environment; (3) flammability properties such as oxygen index, flame spread, and smoke evolution; and (4) selected physical properties. The thermoplastic polymers evaluated include polyphenylene sulfide, polyaryl sulfone, 9,9-bis(4-hydroxyphenyl)-fluorene polycarbonate-poly(dimethylsiloxane) and polyether sulfone. The thermoset polymers evaluated include epoxy, bismaleimide, a modified phenolic, and polyaromatic melamine resin. These resins were primarily used in the fabrication of glass-reinforced prepregs for the construction of experimental panels. Test results and relative rankings of some of the flammability parameters are presented, and the relationship of the molecular structure, char yield, and flammability properties of these polymers are discussed.
The thermochemical and flammability characteristics of laminating resins and composites currently in use and others being considered for use as aircraft interior panels are described. The properties studied included: (1) limiting oxygen index of the composite constituents; (2) fire containment capability of the composite; (3) smoke evolution from the composite; (4) thermogravimetric analysis; (5) composition of the volatile products of thermal degradation; and (6) relative toxicity of the volatile products of pyrolysis. The performance of high-temperature laminating resins such as modified phenolics, polyimides and bismaleimides is compared with the performance of epoxies. The relationship of increased fire safety with the use of polymers with high anaerobic char yield is shown. Processing parameters of the state-of-the-art epoxy resin and the advanced resin composites are detailed.
A burn/impact test apparatus is used to determine the amount of fiber release from carbon fiber composites after burn and impact. The calculation of the theoretical char binder content of the composite is made based on the temperature of the test specimen and the char yield of the resin as determined by thermogravimetric analysis. The test results indicate that carbon fiber release depends on the type of reinforcement used. There was more fiber release with the quasi-isotropic composite made with unidirectional tape than with the woven fabric reinforcement. The amount of fiber release in the impact chamber after burning is coincident with the calculated char binder.
Polyurethane-modified high impact anaerobic adhesives have been chosen for a bonding application where impact cushion is critical. These adhesives meet all the requirements for high rate production and automatic assembly techniques. With aluminum adherends, one selected adhesive cured at room temperature with the recommended activator retained sixty percent of its original impact strength after twenty-six week aging at 100 C. The impact strength aging, the thermogravimetric analysis results, the outgassing data, and other observations made in this work indicate that the adhesives cured by simple heating give a more durable bond than that cured with an activator at room temperature.
Methods for crosslinking N-methyl substituted aromatic polyamides were investigated in an effort to improve the applicability of these polymers as matrix resins for Kavlar trademark fiber composites. High molecular weight polymers were prepared from isophthaloyl dichloride and 4,4'- bis(methylamino)diphenylmethane with varying proportions of the N,N'bispropargyl diamine incorporated as a crosslinking agent. The propargylcontaining diamines were crosslinked thermally and characterized by infrared spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. Attempts were also made to crosslink polyamide films by exposure to ultraviolet light, electron beam, and gamma radiation.
In chamber thermodegradation procedures were used to access the lethality to rats of the pyrolysis/combustion products of three foams, an adhesive backed metallic tape and RTV silicone rubber adhesive sealant used in spacecraft construction. The role of carbon monoxide in the overall pyrolysate toxicity was also investigated. Post exposure observation of the rats, histological evaluation of selected organs, carbon monoxide concentration in the chamber atmosphere during exposure and the percent carboxyhemoglobin in the animals expiring in the chamber are discussed. Thermogravimetric analysis and dosage response results are given. The lethal effect of the RTV silicon appears to be due to physical obstruction of the respiratory system by particulate matter from pyrolysis.
Details are given for the construction and operation of a 101.3 KN/sq meter (1 atmosphere) redox control system. A solid ceramic oxygen electrolyte cell is used to monitor the oxygen fugacity in the furnace. The system consists of a vertical quench gas mixing furnace with heads designed for mounting the electrolyte cell and with facilities for inserting and removing the samples, a simplified version of a gas mixing apparatus, and devices for experiments under controlled rates of change of temperature. A thermogravimetric analysis system employing these techniques of redox control and measurement is also described. The calibration and maintenance of the system are discussed.
Aircraft seat materials were evaluated in terms of their thermal performance. The materials were evaluated using (a) thermogravimetric analysis, (b) differential scanning calorimetry, (c) a modified NBS smoke chamber to determine the rate of mass loss and (d) the NASA T-3 apparatus to determine the thermal efficiency. In this paper, the modified NBS smoke chamber will be described in detail since it provided the most conclusive results. The NBS smoke chamber was modified to measure the weight loss of materials when exposed to a radiant heat source over the range of 2.5 to 7.5 W/cm sq. This chamber has been utilized to evaluate the thermal performance of various heat blocking layers utilized to protect the polyurethane cushioning foam used in aircraft seats. Various kinds of heat blocking layers were evaluated by monitoring the weight loss of miniature seat cushions when exposed to the radiant heat. The effectiveness of aluminized heat blocking systems was demonstrated when compared to conventional heat blocking layers such as neoprene. All heat blocking systems showed good fire protection capabilities when compared to the state-of-the-art, i.e., wool-nylon over polyurethane foam.
The effect on selected polyimide properties when pendant alkyl groups were attached to the polymer backbone was investigated. A series of polymers were prepared using benzophenone tetracarboxylic acid dianhydride (BTDA) and seven different p-alkyl-m,p'-diaminobenzophenone monomers. The alkyl groups varied in length from C(1) (methyl) to C(9) (nonyl). The polyimide prepared from BTDA and m,p'-diaminobenzophenone was included as a control. All polymers were characterized by various chromatographic, spectroscopic, thermal, and mechanical techniques. Increasing the length of the pendant alkyl group resulted in a systematic decrease in glass transition temperature (Tg) for vacuum cured films. A 70 C decrease in Tg to 193 C was observed for the nonyl polymer compared to the Tg for the control. A corresponding systematic increase in Tg indicative of crosslinking, was observed for air cured films. Thermogravimetric analysis revealed a slight sacrifice in thermal stability with increasing alkyl length. No improvement in film toughness was observed.
Measurements were conducted on 7.6 x 7.6 cm samples of polyurethane seat cushion material in a modified National Bureau of Standards smoke density chamber to simulate real life conditions for an onboard aircraft fire or post-crash fire. In this study, a non-flaming heat radiation condition was simulated. Two aluminized polymeric fabrics (Norfab 11HT-26-A and Preox 1100-4) and one neoprene type material in two thicknesses (Vonar 2 and 3) were tested as heat blocking layers to protect the urethane foam from rapid heat degradation. Thermogravimetric analysis and differential scanning calorimetry were performed to characterize thermally the materials tested. It was found that Vonar 2 or 3 provided approximately equal thermal protection to F.R. urethane as the aluminized fabrics, but at a significant weight penalty. The efficiency of the foams to absorb heat per unit mass loss when protected with the heat blocking layer decreases in the heating range of 2.5-5.0 W/sq cm, but remains unchanged or slightly increases in the range of 5.0-7.5 W/sq cm. The results show that at all heat flux ranges tested the usage of a heat blocking layer in aircraft seats significantly improves their thermal performance.
This study evaluated the materials utilized in the flexible joint for possible failure modes. Studies undertaken included effect of temperature on the strength of the system, effect of fatigue on the strength of the system, thermogravimetric analysis, thermochemical analysis, differential scanning calorimeter analysis, dynamic mechanical analysis, and peel test. These studies indicate that if the joint failed due to a materials deficiency, the most likely mode was excessive temperature in the joint. In addition, the joint material is susceptible to fatigue damage which could have been a contributing factor.
Commercial and experimental fire retardants were screened for possible use wiith acrylic printing inks on aircraft interior sandwich panels. The fire retardants were selected according to their physical properties and thermostabilities. Thermostabilities were determined by thermogravimetric analysis and differential scanning calorimetry. A criterion was then established for selecting the more stable agent. Results show that some of the bromine-containing fire retardants are more thermostable than the acrylic ink, alone, used as a control. Also, the bromine-containing fire retardants yield even better limiting oxygen index values when tested after adding carboxy-terminated butadiene acrylonitrile (CTBN) rubber.
Phosphorus containing polyamides and copolyamides were prepared from 1-(dialkoxyphosphinyl)methyl-2,4- and -2,6-diaminobenzenes. The polymers produced were characterized by infrared and proton nuclear magnetic resonance spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. Their thermal properties were compared with those of the corresponding common polyamides. In addition, by determining the limiting oxygen index value of some of these polyamides, their fire resistance was evaluated.
As a part of the investigation of the control system failure Inertial Upper Stage on IUS-1 flight to position a Tracking and Data Relay Satellite (TDRS) in geosynchronous orbit, the materials utilized in the techroll seal are evaluated for possible failure models. Studies undertaken included effect of temperature on the strength of the system, effect of fatigue on the strength of the system, thermogravimetric analysis, thermomechanical analysis, differential scanning calorimeter analysis, dynamic mechanical analysis, and peel test. The most likely failure mode is excessive temperature in the seal. In addition, the seal material is susceptible to fatigue damage which could be a contributing factor.