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Selection and evaluation of candidate adhesives for bonding composites are described. These are based on mechanical property tests (lap shear and flatwise tensile) and processibility. Consideration is given to composite-to-composite, composite-to-titanium, and honeycomb sandwich structures.
The effects of the incorporation of metal ions into various polyimides on polyimide properties are investigated. Polyimide films derived from 3,3',4,4'-benzophenone tetracarboxylic acid dianhydride (BDTA) 3,3'-diaminobenzophenone (m,m'-DABP), 4,4'-diaminobenzophenone (p,p'-DABP) or 4,4'-oxydianiline were prepared with the concurrent addition of approximately 20 metals in a variety of forms. In general, it is found that the films derived from BDTA + p,p'-DABP were brittle and of poor quality, with brittle films also produced in most of the BDTA + m, m'-DABP polyimides regardless of whether the added metal was hydrate or anhydrous. Thermomechanical analysis, torsional braid analysis, thermal gravimetric analysis, infrared spectral analysis and isothermal studies on many of the polyimide films produced indicate that the softening temperature is generally increased upon the addition of metal ions, at the expense of thermal stability, while no changes in chemical functionality are observed. The best system studied in regard to polymer property enhancement appears to be tri(acetylacetonato)aluminum(III) added to the m, m'-DABP polyamide, which has been found to exhibit four times the lap shear strength of the polyimide alone.
The plane strain of adhesively bonded structures which consist of two different orthotropic adherents is considered. Assuming that the thicknesses of the adherends are constant and are small in relation to the lateral dimensions of the bonded region, the adherends are treated as plates. The transverse shear effects in the adherends and the in-plane normal strain in the adhesive are taken into account. The problem is reduced to a system of differential equations for the adhesive stresses which is solved in closed form. A single lap joint and a stiffened plate under various loading conditions are considered as examples. To verify the basic trend of the solutions obtained from the plate theory a sample problem is solved by using the finite element method and by treating the adherends and the adhesive as elastic continua. The plate theory not only predicts the correct trend for the adhesive stresses but also gives rather surprisingly accurate results.
The characterization of addition polyimides with various end caps for adhesive applications at 120-250 C environments is discussed. Oligometric polyimides were prepared from 3,3',4,4'-benzophenone tetracarboxylic dianhydride and 3,3'-methylenedianiline which were end-capped with functionally reactive moities which cause crosslinking when the oligomers are heated to 200-400 C. The syntheses of the oligomers are outlined. The thermolysis of the oligomers was studied by differential scanning calorimetry and the resulting polymers were characterized by differential thermal analysis and adhesive performance. The adhesive data include lap shear strengths on titanium 6-4 adherends both before and after aging for 1000 hours at 121 C and/or 232 C.
Both photoelectron emission and ellipsometry proved successful in detecting silicone contamination on unpainted and epoxy painted metal surfaces such as those of the external tank and the solid rocket booster. Great success was achieved using photoelectron emission (PEE). Panels were deliberately contaminated to controlled levels and then mapped with PEE to reveal the areas and levels that were contaminated. The panels were then tested with regard to adhesive properties. Tapes were bonded over the contaminated and uncontaminated regions and the peel force was measured, or the contaminated panels were bonded (with CPR 483 foam) to uncontaminated panels and made into lap shear specimens. Other panels were bonded and made into wedge specimens for hydrothermal stress endurance tests. Strong adhesion resulted if the PEE signal fell within an acceptance window, but was poor outside the acceptance window. A prototype instrument is being prepared which can automatically be scanned over the external liquid hydrogen tank and identify those regions that are contaminated and will cause bond degradation.
The development effort on the composite beam cap fabricator was completed within cost and close to abbreviated goals. The design and analysis of flight weight primary and secondary beam builder structures proceeded satisfactorily but remains curtailed until further funding is made available to complete the work. The induction fastening effort remains within cost and schedule constraints. Tests of the LARC prototype induction welder is continuing in an instrumented test stand comprised of a Dumore drill press (air over oil feed for variable applied loads) and a dynamometer to measure actual welding loads. Continued testing shows that the interface screening must be well impregnated with resin to ensure proper flow when bonding graphite-acrylic lap shear samples. Specimens prepared from 0.030 inch thick graphite-polyethersulfone are also available for future induction fastening evaluation.
Pretreated and primed Ti 6-4 surfaces were characterized by scanning electron microscopy/energy dispersive analysis of X-rays (SEM/EDAX) and electron spectroscopy for chemical analysis (ESCA). Fractured lap shear bonded Ti 6-4 specimens were also characterized by SEM/EDAX and ESCA. A number of surface techniques were used to characterize Ti02 powders.
An addition polyimide adhesive, LARC 13, was developed which shows promise for bonding both titanium and composites for applications which require service temperatures in excess of 533 K. The LARC 13 is based on an oligomeric bis nadimide containing a meta linked aromatic diamine. The adhesive melts prior to polymerization due to its oligomeric nature, thereby allowing it to be processed at 344 kPa or less. Therefore, LARC 13 is ideal for the bonding of honeycomb sandwich structures. After melting, the resin thermosets during the cure of the nadic endcaps to a highly crosslinked system. Few volatiles are evolved, thus allowing large enclosed structures to be bonded. Preparation of the adhesive as well as bonding, aging, and testing of lap shear and honeycomb samples are discussed.
The results of an investigation into the behavior of adhesively bonded doubler splices of two composite material sandwich panels are presented. The splices are studied from three approaches: analytical; numerical (finite elements); and experimental. Several parameters that characterize the splice are developed to determine their influence upon joint strength. These parameters are: doubler overlap length; core stiffness; laminate bending stiffness; the size of the gap between the spliced sandwich panels; and room and elevated temperatures. Similarities and contrasts between these splices and the physically similar single and double lap joints are discussed. The results of this investigation suggest several possible approaches to improving the strength of the sandwich splices.
A series of polyimides containing silicone elastomers was synthesized in order to study the effects of the elastomer chain length on polymer properties. The elastomer with repeat units varying from n=10 to 105 was chemically reacted into the backbone of an addition polyimide oligomer via reactive aromatic amine groups. Glass transition temperatures of the elastomer and polyimide phases were observed by torsional braid analysis. The elastomer-modified polyimides were tested as adhesives for bonding titanium in order to determine their potential for aerospace applications. Adhesive lap shear tests were performed before and after aging bonded specimens at elevated temperatures.
Research during the report period focused on continued scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) of lap shear samples and flatwise tensile specimens and on the surface characterization of TiO2, Ti 6-4, and Ti powders with particular emphasis on their interaction with primer solutions of both polyphenylquinoxaline and LaRC-13 polyimide. The use of SEM and XPS in the analysis of Ti 6-4 adherend surfaces is described as well as differences in Ti 6-4 surface composition after different chemical pretreatments. Analysis of fractured surfaces is used to established the failure mode. The surface acidity of Ti 6-4 coupons can be established by reflectance visible spectroscopy using indicator dyes.
A chemical vapor deposited tungsten with dispersed carbides was selected as the material for Space Shuttle Orbital Maneuvering and Reaction Control Systems check valve poppets and seats. The selection followed a NASA-sponsored prototype check valve development program utilizing the cutter-seal shell poppet concept. The poppet material is deposited as a coating approximately 0.9 mm thick and fabricated into a shell as a free standing body. The seat material is deposited as a coating 1.1 mm thick on a seat blank, and the cutter seal is machined in the coating. Module tests demonstrated that the material could be ground and lapped to very sharp edges and could cut through typical system contaminants without excessive damage to the sealing surfaces. The material was also determined to be unaffected by exposure to a strongly oxidizing storable propellant.
High-temperature polymers now being developed as adhesives and composite matrices are reviewed, including aromatic polyimides, polybenzimidazoles, polyphenylquinoxalines, nadic end-capped imide oligomers, maleimide end-capped oligomers, and acetylene-terminated imide oligomers. The mechanical properties of laminates based on these resins are reported together with preliminary test results on the adhesive properties for titanium-to-titanium and composite-to-composite lap shear specimens.
In this paper an adhesively bonded lap joint is analyzed by assuming that the adherends are elastic and the adhesive is linearly viscoelastic. After formulating the general problem a specific example for two identical adherends bonded through a three parameter viscoelastic solid adhesive is considered. The standard Laplace transform technique is used to solve the problem. The stress distribution in the adhesive layer is calculated for three different external loads namely, membrane loading, bending, and transverse shear loading. The results indicate that the peak value of the normal stress in the adhesive is not only consistently higher than the corresponding shear stress but also decays slower.
A study was conducted to determine the effects of added elastomers on the thermal stability, adhesive strength, and fracture toughness of LARC-13, a high-temperature addition polyimide adhesive. Various butadiene/acrylonitrile and silicon elastomers were incorporated into the polyimide resin either as physical polyblends, or by chemically reacting the elastomers with the polyimide backbone. Adhesive single lap-shear and T-peel strengths were measured before and after ageing at elevated temperature. A tapered double-cantilever beam specimen was used to determine the fracture toughness of the elastomer-modified polyimide adhesives.
A study has been conducted to determine the effects of added elastomers on the Tg, thermal stability, adhesive strength, and fracture toughness of LARC-13, a high-temperature addition polyimide adhesive. Various butadiene/acrylonitrile and silicone elastomers were incorporated into the polyimide resin (1) as physical polyblends, and (2) by chemically reacting the elastomers with the polyimide backbone. Adhesive single lap-shear and T-peel strengths were measured before and after aging at elevated temperature. A tapered double-cantilever beam specimen was used to determine the fracture toughness of the elastomer-modified polyimide adhesives.
High temperature-resistant adhesive systems were screened for processability, mechanical and physical properties, operational capability at 589 K (600 F), and the ability to produce large area bonds of high quality in fabricating Space Shuttle components. The adhesives consisted primarily of polyimide systems, including FM34B-18, NR-150B2 (DuPont), PMR-15, LARC-13, LARC-160, Thermid 600, and AI-1130L (AMOCA). The processing studies included preparation of polyimide resins, fabrication of film adhesives, development of lay-up and cure procedures, fabrication of honeycomb sandwich panels, and fabrication of mid-plane bonded panels in joints up to 30.5 cm (12 in.) wide. The screening program included tests for tack and drape properties, reticulation and filleting characteristics, ability to produce void-free or low porosity bonds in mid-plane bonded panels, out-time stability, lap shear strength, climbing drum peel strength, and glass transition temperature (Tg). This paper describes the processing methods developed and the test results.
The general plane strain problem of adhesively bonded structures consisting of two different, orthotropic adherends is considered, under the assumption that adherend thicknesses are constant and small in relation to the lateral dimensions of the bonded region, so that they may be treated as plates. The problem is reduced to a system of differential equations for the adhesive stresses which is solved in closed form, with a single lap joint and a stiffened plate under various loading conditions being considered as examples. It is found that the plate theory used in the analysis not only predicts the correct trend for adhesive stresses but gives surprisingly accurate results, the solution being obtained by assuming linear stress-strain relations for the adhesive.