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Polymeric materials thermal degradation kinetic parameters using combined mass spectrometric and thermogravimetric analysis /MS-TGA/
Toxic gases evolved from the thermal oxidative degradation of synthetic or natural polymers in small laboratory chambers or in large scale fire tests are measured by several different analytical methods. Gas detector tubes are used for fast on-site detection of suspect toxic gases. The infrared spectroscopic method is an excellent qualitative and quantitative analysis for some toxic gases. Permanent gases such as carbon monoxide, carbon dioxide, methane and ethylene, can be quantitatively determined by gas chromatography. Highly toxic and corrosive gases such as nitrogen oxides, hydrogen cyanide, hydrogen fluoride, hydrogen chloride and sulfur dioxide should be passed into a scrubbing solution for subsequent analysis by either specific ion electrodes or spectrophotometric methods. Low-concentration toxic organic vapors can be concentrated in a cold trap and then analyzed by gas chromatography and mass spectrometry. The limitations of different methods are discussed.
Silicon carbide (SiC) fiber is a material that may be used in advanced thermal protection systems (TPS) for future aerospace vehicles. SiC fiber's mechanical properties depend greatly on the presence or absence of sizing and its microstructure. In this research, silicon dioxide is found to be present on the surface of the fiber. Electron Spectroscopy for Chemical Analysis (ESCA) and Scanning Electron Microscopy (SEM) show that a thin oxide layer (SiO2) exists on the as-received fibers, and the oxide thickness increases when the fibers are exposed to high temperature. ESCA also reveals no evidence of Si-C bonding on the fiber surface on both as-received and heat treated fibers. The silicon oxide layer is thought to signal the decomposition of SiC bonds and may be partially responsible for the degradation in the breaking strength observed at temperatures above 400 C. The variation in electrical resistivity of the fibers with increasing temperature indicates a transition to a higher band gap material at 350 to 600 C. This is consistent with a decomposition of SiC involving silicon oxide formation.
Thermal exposure effects on the properties of five boron/aluminum composite systems were experimentally investigated. The composite systems were 49 volume percent boron fibers (203 micron diameter) in aluminum-alloy matrices 1100 Al, 2024 Al, 3003 Al, 5052 Al, and 6061 Al. Specimens were thermally exposed up to 10,000 hours at 500 K and 590 K, up to 500 hours at 730 K, and up to 10,000 hours at 500 K and 590 K, up to 500 hours at 730 K, and up to 2000 thermal cycles between 200 K and 590 K. Composite longitudinal and transverse tensile strengths, longitudinal compression strength, and in-plane shear strength were determined. None of the systems was severely degraded by exposure at 590 K. The best performing system was B-2024 Al. Effects of matrix alloys on degradation mechanisms were experimentally investigated. Composite specimens and individual fibers were metallurgically analyzed with a scanning electron microscope and an electron microprobe to determine failure characteristics, chemical element distribution, and reaction layer morphology. Alloying constituents were found to be affect the composite degradation mechanisms as follows: alloys containing iron, but without manganese as a stabilizer, caused increased low-temperature degradation; alloys containing magnesium, iron, or manganese caused increased degradation; and alloys containing copper caused increased fiber strength.
The variation of ultimate tensile strength with thermal treatment of B-Al composite materials and of boron fibers chemically removed from these composites is studied systematically in an attempt to determine the mechanism of the resulting strength degradation. The results indicate that thermally cycling of B-Al represents a more severe condition than equivalent time at temperature. Degradation of composite tensile strength from about 1.3 GN/sq m to as low as 0.34 GN/sq m was observed after 3000 cycles to 420 C for 203-micron B-1100 Al composite. In general, the 1100 Al-matrix composites degraded somewhat more than the 6061 matrix material studied. Measurement of fiber strengths confirmed a composite strength loss due to the degradation of fiber strength. Microscopy indicated a highly flawed fiber surface. On the basis of various thermal-cycling studies and electron diffraction analysis, a mechanism is favored in which B reacts with Al, freshly exposed by cold working during cycling, to form AlB2. The nonuniform interface reaction leads to a highly flawed and weakened B fiber.
The variation of ultimate tensile strength with thermal treatment of B-Al composite materials and of boron fibers chemically removed from these composites in an attempt to determine the mechanism of the resulting strength degradation was studied. Findings indicate that thermally cycling B-Al represents a more severe condition than equivalent time at temperature. Degradation of composite tensile strength from about 1.3 GN/m squared to as low as 0.34 GN/m squared was observed after 3,000 cycles to 420 C for 203 micrometers B-1100 Al composite. In general, the 1100 Al matrix composites degraded somewhat more than the 6061 matrix material studied. Measurement of fiber strengths confirmed a composite strength loss due to the degradation of fiber strength. Microscopy indicated a highly flawed fiber surface.
The effects of isothermal and cyclic exposure on the room temperature axial and transverse tensile strength and dynamic flexural modulus of 35 volume percent and 55 volume percent FP-Al2O3/EZ 33 magnesium composites were studied. The composite specimens were continuously heated in a sand bath maintained at 350 C for up to 150 hours or thermally cycled between 50 and 250 C or 50 and 350 C for up to 3000 cycles. Each thermal cycle lasted for a total of six minutes with a hold time of two minutes at the maximum temperature. Results indicate to significant loss in the room temperature axial tensile strength and dynamic flexural modulus of composites thermally cycled between 50 and 250 C or of composites isothermally heated at 350 C for up to 150 hours from the strength and modulus data for the untreated, as fabricated composites. In contrast, thermal cycling between 50 and 350 C caused considerable loss in both room temperature strength and modulus. Fractographic analysis and measurement of composite transverse strength and matrix hardness of thermally cycled and isothermally heated composites indicated matrix softening and fiber/matrix debonding due to void growth at the interface and matrix cracking as the likely causes of the strength and modulus loss behavior.
The effects of isothermal and cyclic exposure on the room temperature axial and transverse tensile strength and dynamic flexural modulus of 35 volume percent and 55 volume percent FP-Al203/EZ 33 magnesium composites were studied. The composite specimens were continuously heated in a sand bath maintained at 350 C for up to 150 hours or thermally cycled between 50 and 250 C or 50 and 350 C for up to 3000 cycles. Each thermal cycle lasted for a total of six minutes with a hold time of two minutes at the maximum temperature. Results indicate no significant loss in the room temperature axial tensile strength and dynamic flexural modulus of composites thermally cycled between 50 and 250 C or of composites isothermally heated at 350 C for up to 150 hours from the strength and modulus data for the untreated, as-fabricated composites. In contrast, thermal cycling between 50 and 350 C caused considerable loss in both room temperature strength and modulus. Fractographic analysis and measurement of composite transverse strength and matrix hardness of thermally cycled and isothermally heated composites indicated matrix softening and fiber/matrix debonding due to void growth at the interface and matrix cracking as the likely causes of the strength and modulus loss behavior. Previously announced in STAR as N82-21260
Aluminium metal matrix composites with a low cost fiber, e.g. SiC, provide for an attractive combination of high elastic modulus and longitudinal strengths coupled with a low density. SiC (volume fraction 0.55)-aluminum (6061) systems have been studied in order to optimize fiber composite strength and processing parameters. A comparison of two SiC/aluminum composites produced by AVCO and DWA is provided. Fiber properties are shown to alter composite tensile properties and fracture morphology. The room temperature tensile strengths appear to be insensitive to thermal exposures at 500 C up to 150 h. The elastic modulus of the composites also appears to be stable up to 400 C, however variations in the loss modulus are apparent. The fracture morphology reflects the quality of the interfacial bond, fiber strengths and fiber processing.
Since the autoxidative process accounts in part for the degradation of rubber, including aircraft tires, it was felt that a study of the chemiluminescence from unsaturated elastomers could contribute significantly to an understanding of the degradation mechanism. The study revealed similarities in chemiluminescence behavior between four elastomers which were investigated, and it shows that similar oxidation mechanisms occur. Oxidative chemiluminescence was observed from purified samples of cis-1,4-polybutadiene, cis-1,4-polyisoprene, trans-polypentenamer, and 1,2-polybutadiene in an oxygen atmosphere at 25-150 C. The elastomer samples were placed in a 600 watt oven which is equipped with gas inlets for introducing any desired atmosphere. Chemiluminescence emission from the samples was focused with a two inch quartz lens onto the detector of a 12" photomultiplier which is connected to a photon counter. A strip-chart recorder, connected to the counter, permitted automatic data collection. Diagrams of the apparatus are included. The chemical reactions which occurred from the thermal decomposition of the polymer samples are described, and results (and tabulated data) are discussed.
Since the first Mars Sample Return (MSR)-related report published by the Jet Propulsion Laboratory (JPL) in 1974, a series of panels, reports, and white papers have recognized the importance of sample temperature in meeting mission goals and defined a sample maximum temperature (henceforth SMT) limit. The Mars Sample Handling and Requirements Panel (MSHARP, 1999) flatly stated that “[t]he main issue in sample preservation is temperature”. The Mars Exploration Program Analysis Group (MEPAG)’s “Science Priorities for Mars Sample Return” report (2008), declared that “[s]ignificant loss, particularly to biological studies, occurs if samples reach +50°C for three hours ” whereby “scientific objectives related to life goals could be seriously compromised”. Overall, a total of seven panels, white papers, and conference reports adopted a SMT of -40±17°C to preserve samples sufficiently to confidently achieve success in studies of past or present Martian life (see more detail in [5]). In contrast, the Mars 2020 rover (M2020) mission adopted a SMT of +60°C for samples stored on the Martian surface and +50°C for samples retained inside the rover, as stated in a conference poster presented by Beaty et al., 2016. M2020 is currently collecting samples for MSR in tubes. Half of those tubes will be retained within the M2020 rover body (hereafter rover samples, or RS) and half will be deposited on the Martian surface (cached samples or CS), with a currently undetermined number of each collected up to ten years later for return to Earth. CS samples can be expected to experience significantly higher temperatures than RS samples based on their exposed location in sunlight. This work will explore differences in deleterious chemical reaction rates due to thermal environment of both tube types. The findings here should be debated openly and considered when deciding which samples to return to Earth.
Three polymeric materials were evaluated for relative toxicity of their pyrolysis products to rats by inhalation: Y-7683 (LS 200), Y-7684 (Vonar 3 on Fiberglass), and Y-7685 (Vonar 3 on N W Polyester). Criteria employed for assessing relative toxicity were (1) lethality from in-chamber pyrolysis, (2) lethality from an outside-of-chamber pyrolysis MSTL Procedure, and (3) disruption of trained rats' shock-avoidance performance during sub-lethal exposures to in-chamber pyrolysis of the materials.
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The effect of instillation of ultrafine TiO2 particles (10-nm anatase-TiO2 and 12-nm rutile-TiO2 (administered in doses from 60 to 1000 microg/rat and 500 microg/rat, respectively) on the respiratory tract of exposed rats was compared to the effects of larger (250 nm anatase-TiO2 and 220-nm rutile-TiO2 particles (given in doses 500 or 1000 microg/rat and 500 microg/rat, respectively). These effects were also compared to the effects of inhalation of 20-nm and 250-nm anatase-TiO2 particles and inhalation with surrogate gas phase components (HF and HCl). It was found that ultrafine TiO2 particles induced greater inflammatory reaction in the lung, had greater adverse effect on alveolar macrophage-mediated clearance function, and had a greater potential to induce mediators which can adversely affect other lung cells than did larger-sized particles. Inhalation of surrogate gas phase components caused injury only to the upper respiratory tract, in contrast to the ultrafine particles, which affected the deep lung.
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Lunar dust reflectance degradation of thermal control paint on Surveyor 3 TV camera, separating solar radiation effects by analytical model
Thermal oxidative degradation studies were performed on unbranched perfluoroalkylethers at 288 C in oxygen. Metals and alloys studied included Ti, Al, and Ti (4 Al, 4 Mn). The mechanism of degradation was by chain scission. Ti and Al promoted less degradation than Ti (4 Al, 4 Mn). The two inhibitors investigated (a perfluorophenyl phosphine and a phosphatriazine) reduced degradation rates by several orders of magnitude. Both inhibitors were effective for the same duration (75 to 100 hours). The phosphatriazine appeared to provide more surface protection.