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LARC-TPI, an aromatic thermoplastic polyimide, was exposed to an oxygen plasma as a surface pretreatment for adhesive bonding. Chemical and physical changes which occurred in the polyimide surface as a result of the plasma treatment were investigated using X-ray photoelectron spectroscopy (XPS), infrared reflection-absorption spectroscopy (IR-RAS), contact-angle analysis, ellipsometry, and high resolution SEM. A 180-deg peel test with an acrylate-based pressure sensitive adhesive as a flexible adherent was utilized to study the interactions of the plasma-treated polyimide surface with other polymeric materials. The surface characterization and adhesion testing results showed that the oxygen plasma treatment, while creating a more hydrophilic, polar surface, also caused chain scission, resulting in the formation of a weak boundary layer which inhibited adhesion.

Previous work showed that the total number of insects sticking to an aluminum surface was reduced by coating the aluminum surface with elastomers. Due to a large number of possible experimental errors, no correlation between the modulus of elasticity, the elastomer, and the total number of insects sticking to a given elastomer was obtained. One of the errors assumed to be introduced during the road test is a variable insect flux so the number of insects striking one surface might be different from that striking another sample. To eliminate this source of error, the road test used to collect insects was simulated in a laboratory by development of an insect impacting technique using a pipe and high pressure compressed air. The insects are accelerated by a compressed air gun to high velocities and are then impacted with a stationary target on which the sample is mounted. The velocity of an object exiting from the pipe was determined and further improvement of the technique was achieved to obtain a uniform air velocity distribution.

The effect of anodization in NaOH, H2SO4, and amine salts on the surface chemistry of carbon fibers was examined by X-ray photoelectron spectroscopy (XPS). The surfaces of carbon fibers after anodization in NaOH and H2SO4 were examined by scanning transmission electron microscopy (STEM), angular dependent XPS, UV absorption spectroscopy of the anodization bath, secondary ion mass spectrometry, and polar/dispersive surface energy analysis. Hercules AS-4, Dexter Hysol XAS, and Union Carbide T-300 fibers were examined by STEM, angular dependent XPS, and breaking strength measurement before and after commercial surface treatment. Oxygen and nitrogen were added to the fiber surfaces by anodization in amine salts. Analysis of the plasmon peak in the carbon 1s signal indicated that H2SO4 anodization affected the morphological structure of the carbon fiber surface. The work of adhesion of carbon fibers to thermoplastic resins was calculated using the geometric mean relationship. A correlation was observed between the dispersive component of the work of adhesion and the interfacial adhesion.

The results of calorimetric measurements of Ti adherend surfaces are presented. The measurements were carried out after several chemical pretreatments and after fracture of several lap shear samples aged at high temperature. The exact composition of the Ti samples was Ti(6 percent Al-4 percent V). The adhesives used were polyimides and polyphenylquinoxalines (PPQ). Each chemical pretreatment was accompanied by a unique spectroscopic feature which was characterized by XPS, SEM, and specular reflectance infrared spectroscopy. The energetics of the interaction between primer solutions and the Ti adherend were evaluated by microcalorimetry. Changes in the structure of the surface oxide layer upon heating of the adherend were deduced from immersion temperatures of the PI and PPQ solutions. The XPS and SEM data are given is a table.

The role of the interfacial region in determining the bond strength and durability of composite bonds is discussed. The characterization of a variety of carbon fibers including Celion 6000 using both scanning electron microscopy and X-ray photoelectron spectroscopy is discussed. The emphasis is on composite bonding, that is, the adhesive bonding between composites in contrast to fiber-matrix interaction. The primary objective of the research is the characterization of composite surfaces before adhesive bonding and after fracture of bonded specimens. Work done on the analysis of composite samples pretreated in a number of ways prior to bonding is detailed.

The surface properties associated with good adhesive joints were evaluated in terms of application of adhesive bonding in aerospace technology. The physical and chemical nature was determined of Ti and Al adherend surfaces after various surface treatments, and the effects on fracture surfaces of high temperature aging, and variations in amide, anhydride, and solvent during polymer synthesis. The effects were characterized of (1) high temperature during shear strength testing, (2) fiber-reinforced composites as adherends, (3) acid/base nature of adherends, (4) aluminum powder adhesive filler, and (5) bonding pressure.

Several techniques were used to study pretreated Ti 6-4 surfaces including scanning electron microscopy (SEM), electron spectroscopy of chemical analysis (ESCA), and, reflectance visible spectroscopy. Each pretreatment type gave a characteristic surface morphology as seen by SEM. Elemental analysis of the Ti 6-4 surfaces was done using ESCA. Trace residual contaminants from particular chemical pretreatments were identified readily. Results indicate that reflectance visible spectroscopy using indicator dyes placed on Ti 6-4 surfaces appears to be a feasible approach to establish surface acidity. Differences in surface acidity were observed using bromthymol blue on Ti 6-4 surfaces pretreated by two different methods.

The acid-base properties of titanium 6-4 plates (low surface area) were investigated after three different pretreatments, namely Turco, phosphate-fluoride and Pasa-Jell. A series of indicators was used and color changes were detected using diffuse reflectance visible spectroscopy. Electron spectroscopy for chemical analysis was used to examine the indicator on the Ti 6-4 surface. Specular reflectance infra-red spectroscopy was used to study the adsorption of stearic acid from cyclohexane solutions on the Ti 6-4 surface.

Adherend surfaces and fractography were studied using electron spectroscopy for chemical analysis and scanning electron microscopy/energy dispersive analysis of X-rays. In addition, Auger Electron Spectroscopy with depth profiling capability was used. It is shown that contamination of adhesion systems plays an important role not only in determining initial bond strengths but also in the durability of adhesive bonds. It is concluded that the analytical techniques used to characterize and monitor such contamination.

The ability of SEM/EDAX to determine the physical and chemical composition of very small areas was used to study several diverse types of samples representative of NASA-LaRC technology. More systematic investigation was carried out on differences in the results of grit-blasting Ti 6-4 adherends and the presence of extraneous elements, primarily silicon, in some polymer/HT-S fiber composites. Initial results were obtained from a fractured (ILS) short-beam shear specimen, and from Ti 6-4 alloy, before and after a proprietary Boeing anodizing surface preparation for adhesive bonding. Photomicrographs and EDAX spectra were also obtained from new, fractured lap shear strength specimens that employed PPQ and LARC-13 adhesives.

High temperature polymer surface characteristics associated with joint strength were evaluated. Selected samples represented composite adherends, aluminum filler and fiber glass carrier cloth. Detailed analysis of fractured joint surfaces revealed unique characteristics typical of the specific adhesive formulations and test conditions. A fracture mechanism model was developed for correlating macroscopic shear strength and microstructure of fracture surfaces. Applications were made to unpublished data on polyimides and fluoropolymers.