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Aliphatic segments in polyimide backbones achieve low molding temperatures and resistance to solvents. Low molding temperatures in combination with good solvent resistance make these polymers candidates for use in aerospace applications.
Nine new condensation polyimides containing the trifluorophenylethylidene linkage were synthesized by the amic-acid route. Several other polyimides, including some with the hexafluoroisopropylidene linkage, were also prepared as controls. Amic-acid solutions were characterized by determining their inherent viscosities prior to thermal conversion into polyimide films. Glass transition temperatures (T sug g), thermogravimetric analysis (TGA), and isothermal weight loss data were obtained for the films. The films were pulverized into molding powders which, in turn, were thermally processed under pressure into neat resin discs. The discs were also characterized by T sub gs and 316 C and 371 C isothermal weight losses. The film study identified two new polyimides with T sub gs greater that 371 C and two new polyimides with low rates of weight loss. The resin discs exhibited the same overall trends in T sub g and weight loss as the respective films, however the weight loss per unit surface area was always greater, presumably due to voids or to mechanical degradation induced during preparation of the molding powders.
The progress to date on the development of techniques to toughen continuous thermoplastic composites is summarized. The work, using the approach of toughening the polycarbonate composite matrix with rubber particles, has focused on determining the differences between Double Cantilever Beam (DCB) samples molded inhouse and those molded by NASA. Specifically, an effort was made to account for the differences in fracture toughness observed between the various specimens. In addition, preliminary results of tensile dilatometry tests are described; these tests suggest that processes leading to increased volume and enhanced shear banding are occurring within the rubber toughened system. The results of the effort using another approach, the preparation of random block copolycarbonates, are presented. The synthetic route to these species was modified so that higher molecular weights of these materials can be obtained. In addition, an attempt is being made to determine the exact block length or the number of functional groups in the oligomers since this procedure also should lead to high molecular weight materials. Dynamic mechanical analysis of the copolymer prepared so far indicates that the scale of cooperative molecular motion of the PBA polycarbonate at sub-Tg temperatures is larger than five monomer units. Efforts to find a suitable rubber-toughener for a thermoset system (bismaleimides) is also discussed. Included is a description of the various tougheners intended for use or currently being used.
The relationship between the time evolution of ultrasonic longitudinal velocities, measured in the course of the cure of 3501-6 neat and fiber-reinforced resin, and the time evolution of the degree of cure was studied. The resin samples were placed in a mold, one side of which was a graphite plate, while the rest was made of stainless steel. After placing the mold in a press and applying a single-cycle 5-MHz pulse to the transducer bonded to the outer side of the graphite plate, the echo resulting from the resin-graphite interface and the subsequent echoes from within the resin layer were recorded with a 200-MHz, 8-bit digitizer. The degree of cure was calculated from the acoustic response, using the relationships derived by Winfree and Parker (1986). The calculated degree of cure had the expected time dependence, and the agreement between the degree of cure measured for the neat resin and the prepreg was reasonable.
Stereolithography is computer-aided manufacturing technique. Used to make models and molds of electrodes for electrical-discharge machining (EDM). Eliminates intermediate steps in fabrication of plastic model of object used in making EDM electrode to manufacture object or mold for object.
New technique improves melt flow of polyimide. Uses chemical imidization or cyclodehydration techniques that do not cause significant decrease in molecular weight. Process involves dissolution of polyamide acid in amide solvent or mixture of ether and amide solvent at low percentage of solids followed by treatment of this solution with aprotic organic base, such as triethylamine or pyridine, for period of time prior to treatment with organic dehydrating agent. Latter treatments facilitates formation of polyimide. Useful for production of polyimide molding materials. Expected to have widespread application in preparation of easily processed adhesives, molding powders, and matrix resins.
Polyimides from BTDA with m-phenylenediamine and three aliphatic diamines were prepared in cresol and characterized. Characterization tests included compression strength and modulus, stressed solvent resistance, and melt-flow tests. Efforts to reduce the molecular weights of these polymers by either stoichiometric imbalance or phthalic anhydride end capping produced opacity in the polymer moldings when the stoichiometry was less than 99 percent. Use of 2,4-diaminotoluene in place of the m-phenylenediamine allowed clear polymer moldings to be obtained at all stoichiometries by end capping or stoichiometric imbalance. After melt-flow/molecular-weight studies, carbon fabric composites were prepared from three polyimide compositions containing BTDA, 2,4-diaminotoluene and two aliphatic diamines. Flexural strengths of two of the resins were in excess of 689 MPa (100 ksi) at both room temperature and 93 C. The polyimide from BTDA was selected for scale-up and neat resin characterization tests. The Tg of this polymer was 233 C.
The AiResearch Casting Company baseline silicon nitride (92 percent GTE SN-502 Si sub 3 N sub 4 plus 6 percent Y sub 2 O sub 3 plus 2 percent Al sub 2 O sub 3) was characterized with methods that included chemical analysis, oxygen content determination, electrophoresis, particle size distribution analysis, surface area determination, and analysis of the degree of agglomeration and maximum particle size of elutriated powder. Test bars were injection molded and processed through sintering at 0.68 MPa (100 psi) of nitrogen. The as-sintered test bars were evaluated by X-ray phase analysis, room and elevated temperature modulus of rupture strength, Weibull modulus, stress rupture, strength after oxidation, fracture origins, microstructure, and density from quantities of samples sufficiently large to generate statistically valid results. A series of small test matrices were conducted to study the effects and interactions of processing parameters which included raw materials, binder systems, binder removal cycles, injection molding temperatures, particle size distribution, sintering additives, and sintering cycle parameters.
Modified layup schedule counteracts tendency toward delamination. Improved manufacturing process resembles conventional process, except prepregs partially cured laid on mold in sequence in degree of partial cure decreases from mold side to bag side. Degree of partial cure of each layer at time of layup selected by controlling storage and partial-curing temperatures of prepreg according to Arrhenius equation for rate of gel of resin as function of temperature and time from moment of mixing. Differential advancement of cure in layers made large enough to offset effect of advance bag-side heating in oven or autoclave. Technique helps prevent entrapment of volatile materials during manufacturing of fiber/resin laminates.
Fiber-reinforced composite laminates are used in many aerospace and automobile applications. The magnitudes and durations of the cure temperature and the cure pressure applied during the curing process have significant consequences for the performance of the finished product. The objective of this study is to exploit the potential of applying the optimization technique to the cure cycle design. Using the compression molding of a filled polyester sheet molding compound (SMC) as an example, a unified Computer Aided Design (CAD) methodology, consisting of three uncoupled modules, (i.e., optimization, analysis and sensitivity calculations), is developed to systematically generate optimal cure cycle designs. Various optimization formulations for the cure cycle design are investigated. The uniformities in the distributions of the temperature and the degree with those resulting from conventional isothermal processing conditions with pre-warmed platens. Recommendations with regards to further research in the computerization of the cure cycle design are also addressed.
Maneuverable device built around borescope equipped to make impression molds of welded joints in interior surfaces of ducts. Molds then examined to determine degress of mismatch in welds. Inserted in duct, and color-coded handles on ends of cables used to articulate head to maneuver around corners. Use of device fairly easy and requires little training.
Fasteners of carbon/carbon or other fiber/matrix composite materials made by braiding-and-molding process. Preform of braided fibers impregnated with matrix material pressed and cured in internally threaded, split mold to make externally threaded rod. Process costs less, produces stronger fasteners by avoiding breakage of fibers, and adaptable to mass production. Intended for use with ceramic and composite-material structural parts at temperatures approximately greater than 2,500 degrees F (approximately greater than 1,400 degrees C), at which metal fasteners cannot be used.
This is the second annual technical report entitled, Improved Silicon Carbide for Advanced Heat Engines, and includes work performed during the period February 16, 1986 to February 15, 1987. The program is conducted for NASA under contract NAS3-24384. The objective is the development of high strength, high reliability silicon carbide parts with complex shapes suitable for use in advanced heat engines. The fabrication methods used are to be adaptable for mass production of such parts on an economically sound basis. Injection molding is the forming method selected. This objective is to be accomplished in a two-phase program: (1) to achieve a 20 percent improvement in strength and a 100 percent increase in Weibull modulus of the baseline material; and (2) to produce a complex shaped part, a gas turbine rotor, for example, with the improved mechanical properties attained in the first phase. Eight tasks are included in the first phase covering the characterization of the properties of a baseline material, the improvement of those properties and the fabrication of complex shaped parts. Activities during the first contract year concentrated on two of these areas: fabrication and characterization of the baseline material (Task 1) and improvement of material and processes (Task 7). Activities during the second contract year included an MOR bar matrix study to improve mechanical properties (Task 2), materials and process improvements (Task 7), and a Ford-funded task to mold a turbocharger rotor with an improved material (Task 8).
Nine new condensation polyimides containing the phenyltrifluoroethylidene (3F) linkage were synthesized by the amic-acid route. Several other polyimides, including some with hexafluoroisopropylidene (6F) linkage, were also prepared as controls. Amic-acid solutions were characterized by determining their inherent viscosities prior to thermal conversion into polyimide films. Glass transition temperatures (T sub g), thermogravimetric analysis (TGA), and isothermal weight loss data (at 316, 371, and 371 C under 0.5 MPa air pressure) were obtained for the films. The films were pulverized into molding powders which, in turn, were thermally processed under pressure into neat resin disks. The disks were also characterized by T sub g's and 316 and 371 C isothermal weight losses. The film study identified two new polyimides with T sub g's greater than 371 C and two new polyimides with low rates of weight loss. The resin disks exhibited the same overall trends in T sub g and weight loss as the respective films, however the weight loss per unit surface area was always greater, presumably due to molecular degradation induced during preparation of the molding powders. The overall results indicate that polyimides containing the 3F linkage have T sub g's and thermo-oxidative stability comparable to polyimides containing the 6F group. Alternate technology was also shown by the synthesis of two new polyalkyl substituted 3F diamines and five more new 3F polymers. Their potential as photoresists was demonstrated by T sub g advancement after ultraviolet exposure. Last, four U.S. patents on 3F monomers and polymers were issued and up to eight more are pending.
The invention is a pressure rig for repetitive casting of metal. The pressure rig performs like a piston for feeding molten metal into a mold. Pressure is applied to an expandable rubber diaphragm which expands like a balloon to force the metal into the mold. A ceramic cavity which holds molten metal is lined with blanket-type insulating material, necessitating only a relining for subsequent use and eliminating the lengthy cavity preparation inherent in previous rigs. In addition, the expandable rubber diaphragm is protected by the insulating material thereby decreasing its vulnerability to heat damage. As a result of the improved design the life expectancy of the pressure rig contemplated by the present invention is more than doubled. Moreover, the improved heat protection has allowed the casting of brass and other alloys with higher melting temperatures than possible in the conventional pressure rigs.
Friction free bearings at 77 k or higher are possible using the high T(sub c) copper oxide ceramic superconductors. The conventional method for making such bearings is to use a sintered ceramic monolith. This puts great restraints on size, shape and postforming machining. The material is hard and abrasive. It's possible to grind up ceramic superconductors and suspend the granules in a suitable matrix. Mechanical properties improve and are largely dependent on the binder. The Meissner effect is confined to individual grains containing electron vortices. Tracks, rails, levitation areas and bearings can be made this way with conventional plastic molding and extruding machines or by painting. The parts are easily machined. The sacrifice is in bulk electrical conductivity. A percolating wick feel for LN2 can be used to cool remote superconductors and large areas quite effectively. A hollow spheroid or cylinder of superconductor material can be molded with the internal surfaces shielded by the Meissner effect. It might be thought of as the dc magnetic analogue of the Faraday cage and the inside can be called the Meissner space. It's selective. The ac fields are transmitted with minor attenuation. Particle size and distribution have a profound effect on final magnetic and electrical characteristics.
This is the third annual technical report for the program entitled, Improved Silicon Carbide for Advanced Heat Engines, for the period February 16, 1987 to February 15, 1988. The objective of the original program was the development of high strength, high reliability silicon carbide parts with complex shapes suitable for use in advanced heat engines. Injection molding is the forming method selected for the program because it is capable of forming complex parts adaptable for mass production on an economically sound basis. The goals of the revised program are to reach a Weibull characteristic strength of 550 MPa (80 ksi) and a Weibull modulus of 16 for bars tested in 4-point loading. Two tasks are discussed: Task 1 which involves materials and process improvements, and Task 2 which is a MOR bar matrix to improve strength and reliability. Many statistically designed experiments were completed under task 1 which improved the composition of the batches, the mixing of the powders, the sinter and anneal cycles. The best results were obtained by an attritor mixing process which yielded strengths in excess of 550 MPa (80 ksi) and an individual Weibull modulus of 16.8 for a 9-sample group. Strengths measured at 1200 and 1400 C were equal to the room temperature strength. Annealing of machined test bars significantly improved the strength. Molding yields were measured and flaw distributions were observed to follow a Poisson process. The second iteration of the Task 2 matrix experiment is described.
This paper describes the process for manufacturing high-quality test specimens for uses in evaluations of interlaminar tensile strength of laminated composites. The chosen specimen configuration is a curved beam which experiences interlaminar tension in the region of greatest curvature when the beam is subjected to 'opening' forces. The manufacturing process uses a lock-mold tooling approach, the principle of which relies upon the difference in coefficients of thermal expansion between the internal rubber mandrel and the surrounding steel female mold. With this method, compaction pressures above those provided by a typical autoclave can be achieved.