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The concept of introducing organic agents into silicone resins to stabilize these materials against the ravages of ultraviolet radiation is presented. A screening of coating materials, cover materials and ultraviolet screening agents is described. Fabrication processes were developed for the application of thin 25 micrometer coatings to Teflon. Temperature shock and temperature-humidity tests were conducted.
An electron-bombardment argon ion source was used to ion-etch various metals and fluoropolymers. The metal and fluoropolymers were exposed to (0.5 to 1.0)-keV Ar ions at ion current densities of 0.2 to 1.5 mA/sq cm for various exposure times. The resulting surface texture is in the form of needles or spires whose vertical dimensions may range from tenths to hundreds of micrometers, depending on the selection of beam energy, ion current density, and etch time. The bonding of textured surfaces is accomplished by ion-beam texturing mating pieces of either metals or fluoropolymers and applying a bonding agent which wets in and around the microscopic conelike structures. After bonding, both tensile and shear strength measurements were made on the samples. Also tested, for comparison's sake, were untextured and chemically etched fluoropolymers. The results of these measurements are presented in this paper.
Metals and fluoropolymers exposed to 0.5 to 1.0 keV argon ions at current densities of 0.2 to 1.5 mA/sq cm develop surface texturing that increases tensile and shear strength of epoxy bonds. Bonds are 46 to 100 percent stronger than those of chemically etched surfaces. Metals require 3 to 4 hours of bombardment to become properly textured. Fluoropolymers require 5 seconds to 30 minutes. Ion beam will not texture nickel. Unlike chemical treatments, bonding of fluoropolymers can be done days or months after ion treatment.
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.
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.
Sputtered coatings of the refractory metal carbides are of great interest for applications where hard wear-resistant materials are desired. The usefulness of sputtered refractory carbides is often limited in practice by spalling or interfacial separation. In this work improvements in the adherence of refractory carbides on iron, nickel and titanium base alloys were obtained by using oxidation, reactive sputtering or sputtered interlayers to alter the coating-substrate interfacial region. X-ray photoelectron spectroscopy and argon ion etching were used to characterize the interfacial regions, and an attempt was made to correlate adherence as measured in wear tests with the chemical nature of the interface.
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.
Sliding friction experiments were performed in vacuum at room temperature on a plane-type SiC surface in contact with iron-based binary alloys. Multiangular and spherical wear particles were found to form as a result of multipass sliding. The multiangular particles were produced by primary and secondary cracking of the 0001, 10(-)10, and 11(-)20 plane-type cleavage planes under the Hertzian stress field or local inelastic deformation zone. When alloy surfaces are in contact with silicon carbide under a load of 0.2 N, the alloy around the contact area is subjected to stresses that are close to the elastic limit in the elastic deformation region and/or exceed it. It was also found that spherical wear particles may be produced by two mechanisms: a penny-shaped fracture along the circular stress trajectories under the local inelastic deformation zone, and the attrition and fatigue of wear particles.
The polyimide resin, LARC-160, was prepared from diethyl-3, 3', 4,4'-benzophenone tetracarboxylate, ethyl-5-norbornene-2,3-dicarboxylate and Jeffamine AP-22. The imidization reactions of NE and BTDE were studied by HPLC, C-13-NMR and IR. NE imidizes slowly at 12 C; BTDE imidizes when the resin is heated above 100 C. Both imidization reactions proceed directly to the imide. Neither amic acid is present in significant quantities at any stage of the imidization reactions. The monomer mixture was stored at 12 C for periods up to 14 months. The effects of resin aging at this temperature on the chemical composition of the resin monomer mixture and the imidized polymer formed on curing were investigated. Aging the resin monomer mixture has the effect of partially advancing the imidization reaction. The average size of the cured polymer increases slightly with resin age.
The use of scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) in the analysis of Ti 6-4 adherend surfaces is described. Differences in Ti 6-4 surface composition as determined by XPS after different chemical pretreatments are detailed. Analysis of fractured surfaces by SEM/XPS is used to establish the failure mode. The surface acidity of Ti 6-4 coupons can be established by reflectance visible spectroscopy using indicator dyes.
(Previously announced in STAR as N81-28233)
Five samples tested in one cooldown. Holder mounted in testing machine. Submerged in cryogenic liquid held in cryostat. Movable crosshead of testing machine moves gradually downward. Samples placed under tension, one after another, starting with top one; each sample fails in turn before next is stressed.
Current pulses lower resistance of silver-filled epoxies. Capacitive discharge reduces interfacial resistance between aluminum surfaces joined with silver-filled epoxy. Technique offers noninvasive solution to problem of attaching grounding brackets to aluminum honeycomb structures.
The adherence between a ceramic thermal barrier coating and a metal bond coating is improved by ion sputtering a ceramic film on the bond cost. A ceramic thermal barrier coating is then plasma-sprayed onto this primer film. This improves the integrity and strength of the interface between the plasma-sprayed ceramic layer and metallic bond coat which insures stronger adherence between the metal and the ceramic.
A purge and trap technique which was employed to collect and separate the chemicals desorbing from the space shuttle heat protection tiles is described. The instrumentation included a mass spectrometer and gas chromatograph.
The purpose of this project was to determine the chemicals desorbing from the space shuttle heat protection tiles. The original protocol for this project involved direct insertion probe mass spectrometry (DIPMS) analysis of the outgassing products from the tiles. However, this method proved unsatisfactory due to the large number of compounds desorbing from the tiles. A purge and trap technique was then employed to collect and separate the chemicals desorbing from the tiles. The maximum temperature in this analysis was 180 C which is the gas chromatograph fused silica capillary column's temperature limit. The desorption was also carried out at atmospheric pressure with helium as the purge gas. A description of the modified protocol is given. All compounds are tentatively identified.
Strong tape remains sticky over wide temperature range. Strong tape for low temperatures consists of two layers of polyimide tape with layer of reinforcing mesh. Improved tape devised for repairs in space also finds use on Earth in polar regions and in superconducting applications. Tape retains adherence and strength at extreme temperatures, where conventional tapes fail.
The requirements for repair work on Naval aircraft composite wing skins that can be performed under depot conditions (or still worse, under field conditions) are quite restrictive. Equipment that can be used is rather limited as are the available repair space and time. The procedures must be simple enough so that they can be performed satisfactorily by personnel without special knowledge in composite materials technology. Repairs of small holes should not require more than perhaps a short predrying cycle (with heat guns) and a subsequent patch bonding using a heating blanket, held in place by applying a vacuum. However, it has been observed during simulated experimental repair work that the glue lines frequently show a high content of pores and bubbles which are attributed to evaporation of moisture during the curing cycle. (Of course, other volatile materials such as residual solvent would act similarly). The purpose of this paper is to give some detailed analysis of the problem of moisture transport as a function of repair conditions, and to discuss some preliminary work to reduce the effect of moisture by removing moisture chemically with carbodiimides before it reaches a critical level for bubble formations.