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Copoly(imide siloxane) Abhesive Materials with Varied Siloxane Oligomer Length

In this work, low surface energy copoly(imide siloxane)s were synthesized with various siloxane segment lengths. Characterization of these materials revealed that domain formation of the low surface energy component within the matrix was more prevalent for longer siloxane segments as indicated by increased opacity, decreased mechanical properties, and variation of the Tg. Incorporation of siloxanes lowered the polymer s surface energy as indicated by water contact angle values. Topographical modification of these materials by laser ablation patterning further reduced the surface energy, even generating superhydrophobic surfaces. Combined, the contact angle data and particle adhesion testing indicated that copoly(imide siloxane) materials may provide greater mitigation to particulate adhesion than polyimide materials alone. These enhanced surface properties for abhesive applications did result in a reduction of the tensile moduli of the copolymers. It is possible that lower siloxane loading levels would result in retention of the mechanical properties of the polyimide while still affording abhesive surface properties. This hypothesis is currently being investigated. Laser ablation patterning offers further reduction in particle retention as the available surface area for particle adhesion is reduced. Pattern variation and size dependencies are currently being evaluated. For the purposes of lunar dust adhesion mitigation, it is likely that this approach, termed passive due to the lack of input from an external energy source, would not be sufficient to mitigate surface contamination or clean contaminated surfaces for some lunar applications. It is feasible to combine these materials with active mitigation strategies - methods that utilize input from external energy sources - would broaden the applicability of such materials for abhesive purposes. Collaborative efforts along these lines have been initiated with researchers at NASA Kennedy Space Center where experiments are being conducted involving a series of embedded electrodes within polymeric matrices.

Wohl, Christoper J.

Adhesively bonded joints: Testing, analysis, and design; Proceedings of the International Symposium, Baltimore, MD, Sept. 10-12, 1986

The papers contained in this volume provide an overview of the state of the art of testing, analysis, and design of adhesively bonded joints. The papers are grouped in the following sections: mechanical testing, stress analysis, failure mechanisms, and design and durability. Specific topics discussed include determination and verification of elastic parameters for adhesives; factors influencing elastic stresses in double cantilever beam specimens; special mixed finite elements for interfacial stress analysis of adhesively bonded joints; debonding characteristics of adhesively bonded woven Kevlar composites; and environmental durability of adhesively bonded joints.

Johnson, W. S.

Criterion for mixed mode fracture in composite bonded joints

A study was undertaken to characterize the debond growth mechanism of adhesively bonded composite joints under mode I, mixed mode I-II, and mode II static loadings. The bonded system consisted of graphite-epoxy composite adherends bonded with a toughened epoxy adhesive. The mode I, mode II and mixed mode I-II fracture energies of the tested adhesives were found to be equal to each other. The criterion for mixed mode fracture in composite bonded joints was found.

Mall, S.

Criterion for mixed mode fracture in composite bonded joints

A study was undertaken to characterize the debond growth mechanism of adhesively bonded composite joints under mode I, mixed mode I-II, and mode II static loadings. The bonded system consisted of graphite/epoxy (T300/5208) composite adherends bonded with a toughened epoxy (EC 3445) adhesive. The mode I, mode II and mixed-mode I-II fracture energies of the tested adhesive were found to be equal to each other. Furthermore, the criterion for mixed mode fracture in composite bonded joints was determined.

Mall, S.

Tensile and shear strength of adhesives

This experiment is conducted in a freshman-level course: Introduction to Engineering Materials. There are no prerequisites for the course although students should have some knowledge of basic algebra. The objectives are to tension and shear test adhesives and to determine the tensile and shear properties of adhesives. Details of equipment of procedure are given.

Stibolt, Kenneth A.

Coating Reduces Ice Adhesion

The Shuttle Ice Liberation Coating (SILC) has been developed to reduce the adhesion of ice to surfaces on the space shuttle. SILC, when coated on a surface (foam, metal, epoxy primer, polymer surfaces), will reduce the adhesion of ice by as much as 90 percent as compared to the corresponding uncoated surface. This innovation is a durable coating that can withstand several cycles of ice growth and removal without loss of anti-adhesion properties. SILC is made of a binder composed of varying weight percents of siloxane(s), ethyl alcohol, ethyl sulfate, isopropyl alcohol, and of fine-particle polytetrafluoroethylene (PTFE). The combination of these components produces a coating with significantly improved weathering characteristics over the siloxane system alone. In some cases, the coating will delay ice formation and can reduce the amount of ice formed. SILC is not an ice prevention coating, but the very high water contact angle (greater than 140 ) causes water to readily run off the surface. This coating was designed for use at temperatures near -170 F (-112 C). Ice adhesion tests performed at temperatures from -170 to 20 F (-112 to -7 C) show that SILC is a very effective ice release coating. SILC can be left as applied (opaque) or buffed off until the surface appears clear. Energy dispersive spectroscopy (EDS) and x-ray photoelectron spectroscopy (XPS) data show that the coating is still present after buffing to transparency. This means SILC can be used to prevent ice adhesion even when coating windows or other objects, or items that require transmission of optical light. Car windshields are kept cleaner and SILC effectively mitigates rain and snow under driving conditions.

Smith, Trent

Effects of cyclical environments on high-performance multi-layer insulation materials.

Results of a test program designed to determine the effects of 100 temperature and compressive loading cycles on several multilayer insulation materials and composites. A total of four reflector materials, four separator materials, eight face-sheet systems, and one fastener material were subjected to 100 temperature cycles from -320 to 400 or 650 F. Generic types of materials studied included Mylar, Kapton, Dacron, Nomex, and Beta Glass. The temperature cycling was followed by visual inspection, metal adhesion tests on the reflectors, and tensile tests of the face sheets, fastener, and separators. A total of six composites were subjected to compressive cycles between zero and 0.15 psi, and density changes were measured. Application of the experimental results to the shuttle orbiter is discussed.

Krause, D. R.

Coupons (mini-modules) experimental data

Adhesion testing results on mini-module coupons (cell/encapsulant/glass laminates) that were aged under the different accelerated aging conditions (outlined more in the DataHub URL).

accelerated aging

A water blown urethane insulation for use in cryogenic environments

Thermal Protection Systems (TPS) of NASA's Space Shuttle External Tank include polyurethane and polyisocyanurate modified polyurethane foam insulations. These insulations, currently foamed with CFC 11 blowing agent, serve to maintain cryogenic propellant quality, maintain the external tank structural temperature limits, and minimize the formation of ice and frost that could potentially damage the ceramic insulation on the space shuttle orbiter. During flight the external tank insulations are exposed to mechanical, thermal and acoustical stresses. TPS must pass cryogenic flexure and substrate adhesion tests at -253 C, aerothermal and radiant heating tests at fluxes up to approximately 14 kilowatts per square meter, and thermal conductivity tests at cryogenic and elevated temperatures. Due to environmental concerns, the polyurethane insulation industry and the External Tank Project are tasked with replacing CFC 11. The flight qualification of foam insulations employing HCFC 141b as a foaming agent is currently in progress; HCFC 141b blown insulations are scheduled for production implementation in 1995. Realizing that the second generation HCFC blowing agents are an interim solution, the evaluation of third generation blowing agents with zero ozone depletion potential is underway. NASA's TPS Materials Research Laboratory is evaluating third generation blowing agents in cryogenic insulations for the External Tank; one option being investigated is the use of water as a foaming agent. A dimensionally stable insulation with low friability, good adhesion to cryogenic substrates, and acceptable thermal conductivity has been developed with low viscosity materials that are easily processed in molding applications. The development criteria, statistical experimental approach, and resulting foam properties will be presented.

Blevins, Elana

Effect of metallurgical structure and properties on adhesion and friction behavior of cobalt alloys

The metallurgical structure and some of the mechanical properties of two cobalt alloys, cobalt-50% iron and cobalt-25% molybdenum-10% chromium, were determined under various heat treated conditions. The mechanical properties of the bcc disordered Co-50Fe alloy, which was found to be very brittle, indicated an exceedingly low fracture strength, low hardness, and very weak grain boundary strength. Ordering by suitable heat treatment only produced a more brittle material with a lower fracture strength and a slightly higher hardness value. Work hardening was found to produce a finer grain structure and a greater grain boundary strength. Tensile properties were examined. It was found that the Co-25Mo-10Cr alloy was difficult to place in the alpha Co solid solution condition, which limited the ability to use precipitation as a hardening reaction. Over two hundred adhesion cycles from zero contact load, to maximum load, to fracture were conducted between couples for each of the above alloys in an ultrahigh vacuum system which would permit the sample surfaces to be cleaned of all contaminant layers. In the Co-50Fe case, the calculated fracture stress from the adhesion tests showed values in the range of 80 to 150 k.s.i., which is about ten times greater than the values from tension tests.

Keller, D. V., Jr.

Graphite/Polyimide Composites

Technology developed under the Composites for Advanced Space Transportation System Project is reported. Specific topics covered include fabrication, adhesives, test methods, structural integrity, design and analysis, advanced technology developments, high temperature polymer research, and the state of the art of graphite/polyimide composites.

Dexter, H. B.

Phase 2 of the array automated assembly task for the low cost silicon solar array project

Studies were conducted on several fundamental aspects of electroless nickel/solder metallization for silicon solar cells. A process, which precedes the electroless nickel plating with several steps of palladium plating and heat treatment, was compared directly with single step electroless nickel plating. Work was directed toward answering specific questions concerning the effect of silicon surface oxide on nickel plating, effects of thermal stresses on the metallization, sintering of nickel plated on silicon, and effects of exposure to the plating solution on solar cell characteristics. The process was found to be extremely lengthy and cumbersome, and was also found to produce a product virtually identical to that produced by single step electroless nickel plating, as shown by adhesion tests and electrical characteristics of cells under illumination.

Petersen, R. C.

Surfaces

Techniques for the characterization of surface cleanliness and roughness for predicting the quality of an adhesive bond are outlined. Generally, smooth surfaces are only available from cleavage of crystalline materials along a natural cleavage plane. Films must be deposited on metal surfaces to achieve the same smoothness. Once the surfaces are clean, however, reaction with the ambient atmosphere becomes likely through diffusive and absorption processes, producing asperities. Electron diffraction, Auger electron, and X ray emission spectroscopy are used to characterize surface condition. Once the surface is observed to be clean, the application of an adhesive will usually prohibit separation along the adhesive; separation is then confined to the weaker of the two materials. Finally, the use of polytetrafluorothylene adhesive to test the adhesion between polymers and metal surfaces is described.

Buckley, D. H.

Pulsed excimer laser processing

The status of pulsed excimer laser processing of PV cells is presented. The cost effective feasibility of fabricating high efficiency solar cells on Czochralski wafers using a pulsed excimer laser for junction formation, surface passivation, and front metallization. Laser annealing results were promising with the best AR coated cell having an efficiency of 16.1%. Better results would be expected with larger laser spot size because there was some degradation in open circuit voltage caused by laser spot overlap and edge effects. Surface heating and photolytic decomposition by the laser was used to deposit tungsten from the reaction of tungsten hexafluoride and hydrogen. The line widths were 5 to 10 mils, and the depositions passed the tape adhesion test. Thinner lines are practical using an optimized optical system.

Wong, D.

Interfacial adhesion: Theory and experiment

Adhesion, the binding of different materials at an interface, is of general interest to many branches of technology, e.g., microelectronics, tribology, manufacturing, construction, etc. However, there is a lack of fundamental understanding of such diverse interfaces. In addition, experimental techniques generally have practical objectives, such as the achievement of sufficient strength to sustain mechanical or thermal effects and/or have the proper electronic properties. In addition, the theoretical description of binding at interfaces is quite limited, and a proper data base for such theoretical analysis does not exist. This presentation will review both experimental and theoretical aspects of adhesion in nonpolymer materials. The objective will be to delineate the critical parameters needed, governing adhesion testing along with an outline of testing objectives. A distinction will be made between practical and fundamental objectives. Examples are given where interfacial bonding may govern experimental consideration. The present status of theory is presented along wiith recommendations for future progress and needs.

Ferrante, John

Interfacial adhesion - Theory and experiment

Adhesion, the binding of different materials at an interface, is of general interest to many branches of technology, e.g., microelectronics, tribology, manufacturing, construction, etc. However, there is a lack of fundamental understanding of such diverse interfaces. In addition, experimental techniques generally have practical objectives, such as the achievement of sufficient strength to sustain mechanical or thermal effects and/or have the proper electronic properties. In addition, the theoretical description of binding at interfaces is quite limited, and a proper data base for such theoretical analysis does not exist. This presentation will review both experimental and theoretical aspects of adhesion in nonpolymer materials. The objective will be to delineate the critical parameters needed, governing adhesion testing along with an outline of testing objectives. A distinction will be made between practical and fundamental objectives. Examples are given where interfacial bonding may govern experimental consideration. The present status of theory is presented along with recommendations for future progress and needs.

Ferrante, John

Preliminary evaluation of adhesion strength measurement devices for ceramic/titanium matrix composite bonds

The adhesive bond between ceramic cement and a titanium matrix composite substrate to be used in the National Aerospace Plane program is evaluated. Two commercially available adhesion testers, the Sebastian Adherence Tester and the CSEM REVETEST Scratch Tester, are evaluated to determine their suitability for quantitatively measuring adhesion strength. Various thicknesses of cements are applied to several substrates, and bond strengths are determined with both testers. The Sabastian Adherence Tester has provided limited data due to an interference from the sample mounting procedure, and has been shown to be incapable of distinguishing adhesion strength from tensile and shear properties of the cement itself. The data from the scratch tester has been found to be difficult to interpret due to the porosity and hardness of the cement. Recommendations are proposed for a more reliable adhesion test method.

Pohlchuck, Bobby