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Heat and chemical resistant polymers with triazine crosslinks are prepared by thermal condensation reactions to form 1,2,4-oxdiazole linkages. They are compounded with variety of fillers, extenders, and modifiers for numerous applications in which stability, impermiability to liquids and gases, good plasticity, and elasticity or rigidity are important.
Nine inch diameter samples of the material which will provide thermal and acoustic protection between the nozzle and outer skirt on the space shuttle solid rocket boosters were subjected to heating tests to determine the porosity of the material and the thermal response to a step change in heating. For the porosity measurements a steady state flow of air at 70 F, 500 F, and 1000 F was passed through a sample of the curtain material and measurements of the flow rates were made at different pressure drops across the sample. For the transient measurements, a sample of the curtain material was subjected to a step change in temperature as air was passed through the sample. Measurements of the heat flow through the sample were made as a function of time after the input of the heat pulse. The sample consisted of three layers of curtain panels. Each panel was made of combinations of quartz and fiberglass cloth between which a fiberfrax filler material had been stitched. The hardware design and test procedures were described. Data are provided in engineering units for the flow conditions and and temperatures at which measurements were conducted.
In-depth gap heating ratios for Orbiter RSI tile sidewalls were predicted based on near steady state temperature measurements obtained from double wedge model tests. An analysis was performed to derive gap heating ratios which would result in the best fit of test data; provide an assessment of open gap response, and supply the definition of gap filler requirements on the Orbiter. A comparison was made of these heating ratios with previously derived ratios in order to verify the extrapolation of the wing glove data to Orbiter flight conditions. The analysis was performed with the Rockwell TPS Multidimensional Heat Conduction Program for a 3-D, 2.0-inch thick flat RSI tile with 255 nodal points. The data from 14 tests was used to correlate with the analysis. The results show that the best-fit heating ratios at the station farthest upstream on the model for most gap depths were less than the extrapolated values of the wing glove model heating ratios. For the station farthest downstream on the model, the baseline heating ratios adequately predicted or over-predicted the test data.
The results of a study to determine the degree to which the ductility and tensile properties of peaked welds could be enhanced by removing the reinforcing bead and fairing the weld nugget into the adjacent parent metal are presented. The study employed 2219-T87 aluminum alloy plate, tungsten inert gas (TIG) welding, and 2319 filler wire. The study concluded that significant improvements in peak weld, ultimate strength, and ductility can be obtained through removal and fairing of the weld reinforcing bead. The specimens so treated and tested in this program exhibited ultimate strength improvements of 2 to 3 percent for peak angles of 5.8 to 10 degrees and 10 to 22 percent for welds with peak angles of 11.7 to 16.9 degrees. It was also determined that removal of the weld bead enhanced the ability of peaked welds to straighten when exposed to cyclic loading at stress levels above the yield strength.
Triazine compounds and cross-linked polymer compositions are made by heating aromatic nitriles to a temperature in the range of from about 100 C to about 700 C, and preferably in the range of from about 200 C to about 350 C, in the presence of a catalyst or mixture of catalysts selected from one or more of the following groups: (1) organic sulfonic and sulfinic acids, (2) organic phosphonic and phosphinic acids, and (3)metallic acetylacetonates, at a pressure in the range of from about atmospheric pressure to about 10,000 psi and preferably in the range of from about 200 psi to about 750 psi. Aromatic nitrile-modified (terminated and/or appended) imide, benzimidazole, imidazopyrrolone, quinoxaline, and other condensation type prepolymers or their precopolymers are made which are trimerized with or without a filler by the aforementioned catalytic trimerization process into triaryl-s-triazine ring containing or cross-linked polymeric or copolymeric products useful in applications requiring high thermal-oxidative stability and high performance structural properties at elevated temperatures.
The research to provide a mechanism for dissipation of impact energy in filled polymers by using fillers with a low modulus coating is reported which will dissipate energy through shearing and crazing instead of fracture. The approach offers the advantages of low cost, low toxicity, and applicability to various resins.
Density, dc electrical resistivity, thermal conductivity, and linear thermal expansion are measured for arc-melted rod-shaped samples of binary eutectics of Zr, Hf, Ru, Nb, Ir, Mo, Ta, Os, Re, and W selected as very-low-pressure braze fillers for thermionic converters. The first two properties are measured at 296 K for Zr-21.7 at% Ru, Zr-13 wt% W, Zr-19 wt% W, Zr-22.3 at% Nb, Nb-66.9 at% Ru, Hf-25.3 wt% Re, Zr-25.7 at% Ta, Hf-22.5 at% W, and Nb-35 wt% Mo. The last property is measured from 293 K to 2/3 melting point for specified alloys of different compositions. Resistivities of 0.000055 to 0.000181 ohm-cm are observed with the alloys having resistivities about ten times that of the less resistive constituent metal and about three times that of the more resistive constituent metal, except for Zr-19 wt% W and Nb-35 wt% Mo (greater resistivities). Thermal expansion coefficients vary from 0.000006 to 0.0000105/K. All brazes exhibit linear thermal expansion near that of their constituent metals.
This paper reports on an investigation of the concept of modifying the thermal performance of filled polymers through a minor compositional change (presently by coating the filler). The fire-safety of construction materials and the instability of solid rockets are used as examples. A theory is developed which shows that vast improvements are possible by controlling thermal conductivity. Experiments are described that show the weight loss and smoke density in the NBS smoke-density chamber of fiberglass-reinforced epoxy panels, and the instability trends of an AP-HTPB propellant fired in an L-Star rocket motor. The feasibility of tailoring thermal behavior to suit each particular need is demonstrated.
Thermally-stable, fire-resistant polyimide foams developed for use as fire protection in aircraft, spacecraft and ground applications are presented. Polyimide precursors, synthesized by the reaction of 3, 3', 4, 4'-benzophenone tetracarboxylic acid dianhydride with a mixture of two diamines, can be processed into foams by indirect or direct heating techniques. Flexible resilient foams and thermal acoustical foams produced by the microwave heating of polyimide precursors are shown to conform to requirements for aircraft seating foams and thermal and acoustical insulation materials, respectively. Rigid polyimide foams reinforced by carbon mat, chopped carbon mat and chopped glass strand fillers and prepared by the microwave heating of a continuous mat, followed by its compression, or by filling a honeycomb structure with low density foam, are found to exhibit outstanding fire resistance and have mechanical properties approaching those desired for structural materials.
Procedure permits mounting of heavy parts to surface of composite beams without appreciably weakening beam web. Web is split and held apart in region where attachment is to be made by lightweight precast foam filler. Bolt hole penetrates foam rather than web, and is secured by barrelnut in transverse bushing through web.
Resilient baglike seal tolerates thousand-degree temperatures and accommodates small changes in gap size without losing gas-barrier properties; at same time, it maintains smooth aerodynamic surface across gap. Seal includes alumina filler backed by metal plate. Alumina-filled envelope is easily handled and installed, and can be used in high-temperature industrial processes like coal gasification and liquefaction.
Need for lightweight flame-resistant, nonsmoking materials in interiors of spacecraft has spawned family of foams that could find applications in aircraft and other vehicles. Polyimide-based foams are being developed as resilient fillers for seat cushions, as rigid, low-density wall panels, as high-strength sheets for floors, and as thermal and acoustical insulation.
Modified polyimide-polymer resins are precursors for new family of resilient fire-resistant foams. Terpolyimide foams containing long-chain aliphatic diamines withstand 50,000 cycles of compression over a 200 pound load - an equivalent of 3 years of continuous use as seat cushion filler.
Process that combines microwave foaming and curing of polyimide precursors in single step produces fire-resistant foam slabs of much larger volume than has previously been possible. By adding selected conductive fillers to powder precursors and by using high-power microwave oven, foam slabs with dimensions in excess of 61 by 61 by 7.6 cm are made. Typical foaming and curing and curing time is 35 minutes in microwave oven with additional 1 to 2 hour postcure in conventional oven.
Previous techniques for fabricating rigid fire-resistant polyimide foams by compressing already-foamed precursor have been supplanted by one-step constrained-rise process. Precursor mixed with reinforcing fillers is placed between rigid substrates that constrain expansion of foam as it is heated by microwave energy. Process works for both liquid and powder precursors and can also be adapted to attach woven fiberglass skins at same time prcursor is being foamed.
Tetraethyl orthosilicate (TEOS) mixture fills chips and cracks in glazed tile surface. Filler is made by mixing hydrolyzed TEOS, silicon tetraboride powder, and pulverized tile material. Repaired tiles survived testing by intense acoustic emissions, arc jets, and intense heat radiation. Repair is reliable and rapid, performed in 1-1 1/2 hours with tile in any or orientation.
Graphite fiber reinforced resin matrix composites were subjected to controlled burning conditions to determine their burning characteristics and fiber retention properties. Small samples were burned with a natural gas fired torch to study the effects of fiber orientation and structural flaws such as holes and slits that were machined into the laminates. Larger laminate samples were burned in a modified heat release rate calorimeter. Unidirectional epoxy/graphite and polyimide/graphite composites and boron powder filled samples of each of the two composite systems were burn tested. The composites were exposed to a thermal radiation of 5.3 Btu/sq ft-sec in air. Samples of each of the unfilled composite were decomposed anaerobically in the calorimeter. Weight loss data were recorded for burning and decomposition times up to thirty-five minutes. The effects of fiber orientation, flaws, and boron filler additives to the resins were evaluated. A high char forming polyimide resin was no more effective in retaining graphite fibers than a low char forming epoxy resin when burned in air. Boron powder additions to both the polyimide and the epoxy resins stabilized the chars and effectively controlled the fiber release.
The shuttle orbiter relies primarily on a reusable surface insulation (RSI) thermal protection system (TPS). The RSI is very efficient in its thermal performance; however, the RSI tile system has shown poor mechanical integrity. The state-of-the-art of the ablative TPS is reviewed, and an assessment made of the ablator's readiness for use on the shuttle orbiter. Unresolved technical issues with regard to the ablative TPS are identified. Short time, highly focused analytical and experimental programs were initiated to: (1) identify candidate ablation materials; (2) assess the data base for these materials; (3) evaluate the need and kind of waterproof coating; (4) calculate thermal and other stresses in an ablator tile; (5) identify an acceptable ablator/RSI tile joint filler; and (6) assess the sensitivity of the ablator to sequential heat pulses. Results from some of these programs are discussed.