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NASA NTRS2005

High-Temperature Structures, Adhesives, and Advanced Thermal Protection Materials for Next-Generation Aeroshell Design

The next generation of planetary exploration vehicles will rely heavily on robust aero-assist technologies, especially those that include aerocapture. This paper provides an overview of an ongoing development program, led by NASA Langley Research Center (LaRC) and aimed at introducing high-temperature structures, adhesives, and advanced thermal protection system (TPS) materials into the aeroshell design process. The purpose of this work is to demonstrate TPS materials that can withstand the higher heating rates of NASA's next generation planetary missions, and to validate high-temperature structures and adhesives that can reduce required TPS thickness and total aeroshell mass, thus allowing for larger science payloads. The effort described consists of parallel work in several advanced aeroshell technology areas. The areas of work include high-temperature adhesives, high-temperature composite materials, advanced ablator (TPS) materials, sub-scale demonstration test articles, and aeroshell modeling and analysis. The status of screening test results for a broad selection of available higher-temperature adhesives is presented. It appears that at least one (and perhaps a few) adhesives have working temperatures ranging from 315-400 C (600-750 F), and are suitable for TPS-to-structure bondline temperatures that are significantly above the traditional allowable of 250 C (482 F). The status of mechanical testing of advanced high-temperature composite materials is also summarized. To date, these tests indicate the potential for good material performance at temperatures of at least 600 F. Application of these materials and adhesives to aeroshell systems that incorporate advanced TPS materials may reduce aeroshell TPS mass by 15% - 30%. A brief outline is given of work scheduled for completion in 2006 that will include fabrication and testing of large panels and subscale aeroshell test articles at the Solar-Tower Test Facility located at Kirtland AFB and operated by Sandia National Laboratories. These tests are designed to validate aeroshell manufacturability using advanced material systems, and to demonstrate the maintenance of bondline integrity at realistically high temperatures and heating rates. Finally, a status is given of ongoing aeroshell modeling and analysis efforts which will be used to correlate with experimental testing, and to provide a reliable means of extrapolating to performance under actual flight conditions. The modeling and analysis effort includes a parallel series of experimental tests to determine TSP thermal expansion and other mechanical properties which are required for input to the analysis models.

Collins, Timothy J.↗

NASA NTRS1999

Ultrasonic Nondestructive Characterization of Adhesive Bonds

Adhesives and adhesive joints are widely used in various industrial applications to reduce weight and costs, and to increase reliability. For example, advances in aerospace technology have been made possible, in part, through the use of lightweight materials and weight-saving structural designs. Joints, in particular, have been and continue to be areas in which weight can be trimmed from an airframe through the use of novel attachment techniques. In order to save weight over traditional riveted designs, to avoid the introduction of stress concentrations associated with rivet holes, and to take full advantage of advanced composite materials, engineers and designers have been specifying an ever-increasing number of adhesively bonded joints for use on airframes. Nondestructive characterization for quality control and remaining life prediction has been a key enabling technology for the effective use of adhesive joints. Conventional linear ultrasonic techniques generally can only detect flaws (delamination, cracks, voids, etc) in the joint assembly. However, more important to structural reliability is the bond strength. Although strength, in principle, cannot be measured nondestructively, a slight change in material nonlinearity may indicate the onset of failure. Furthermore, microstructural variations due to aging or under-curing may also cause changes in the third order elastic constants, which are related to the ultrasonic nonlinear parameter of the polymer adhesive. It is therefore reasonable to anticipate a correlation between changes in the ultrasonic nonlinear acoustic parameter and the remaining bond strength. It has been observed that higher harmonics of the fundamental frequency are generated when an ultrasonic wave passes through a nonlinear material. It seems that such nonlinearity can be effectively used to characterize bond strength. Several theories have been developed to model this nonlinear effect. Based on a microscopic description of the nonlinear interface binding force, a quantitative method was presented. Recently, a comparison between the experimental and simulated results based on a similar theoretical model was presented. A through-transmission setup for water immersion mode-converted shear waves was used to analyze the ultrasonic nonlinear parameter of an adhesive bond. In addition, ultrasonic guided waves have been used to analyze adhesive or diffusion bonded joints. In this paper, the ultrasonic nonlinear parameter is used to characterize the curing state of a polymer/aluminum adhesive joint. Ultrasonic through-transmission tests were conducted on samples cured under various conditions. The magnitude of the second order harmonic was measured and the corresponding ultrasonic nonlinear parameter was evaluated. A fairly good correlation between the curing condition and the nonlinear parameter is observed. The results show that the nonlinear parameter might be used as a good indicator of the cure state for adhesive joints.

Qu, Jianmin↗

NASA NTRS1969

Apollo 6, Anomaly Report No. 6: Abnormal Structural Performance During Launch Phase

Approximately 2 minutes 13 seconds after lift-off of the Apollo 6 mission, abrupt changes of strain, vibration, and acceleration measurements were indicated in the S-IVB, instrument unit, adapter, lunar module, and command and service modules; photographs showed objects coming from the area of the adapter. The adapter, however, continued to sustain the required loads with no impairment of the mission. The investigation was first focused upon the understanding of the coupled vibration modes and characteristics of the launch vehicle and spacecraft.' Extensive test programs were conducted. It was eventually concluded that the adapter failure was not caused by vibration. Extensive study of the airborne photography and other evidence indicated that a large area of the adapter had lost inner facesheet from the honeycomb sandwich panels. Loads and stresses resulting from vibration were determined to be insufficient to initiate such a failure. The investigation was then directed toward determining the range of pressures that could have been trapped in the Apollo 6 adapter sandwich panels, and toward determining the tolerance of the panels to withstand pressure with various degrees of flaws such as adhesive voids and facesheet dents. The degradation effects of moisture and heat exposure on the adhesive strength were also studied and tested. These tests and analyses led to the conclusion that pressure internal to the sandwich panels could have caused the failure, if a large flaw existed. The pressure buildup would have been caused by aerodynamic heating effects on air and moisture trapped in the panel. The probable cause of the failure was found in the original ultrasonic inspection scan record of the affected adapter panel. In the center of the region where the adapter failed, horizontally along the station 709 panel splice, the record contained two thick anomalous lines extending several feet. Without an X-ray record of this region, the significance of this particular scan record cannot be fully understood. However, since all other evidence had indicated that the adhesive had to be weakened in a rather large area to initiate the failure, the investigation was focused intently upon the station 709 splices of other adapters. Sufficient information was developed to verify that deficient assembly techniques have consistently resulted in abnormalities in the structure at this station. These abnormalities were identified in adapters 12, 13, 14, 15, and 16. Before the splice abnormalities were pinpointed, corrective action was taken to reduce pressure "buildup in the honeycomb panels and to reduce heat degrading effects on the adhesive. This was done by drilling vent holes in the inner facesheet and covering the outer facesheet with cork. The adapters having identified abnormalities in the station 709 splice are being repaired, and the contractor is investigating ways of avoiding these -abnormalities in panels yet to be bonded.

Source record↗

NASA NTRS1973

Cyclic debonding of adhesive joints: Data report

Static and fatigue loading tests of bonded lap joints were conducted. The specimens were designed to fail in the bondline and all fatigue tests included monitoring the crack growth to failure. Detailed crack length readings for 106 fatigue specimens are provided.

Hoffman, D. J.↗

NASA NTRSDate not supplied

Characterization of Microbe Resistant Coatings for Use in the ISS Water System

The ISS is a highly controlled environment; however, there are still microbes on it that astronauts bring from their own microbiome. Once within the ISS water treatment system, these microbes not only pose a health risk for astronauts, but they can form biofilms, causing material degradation and system failure. Due to their protective structure, biofilms are notoriously resistant to disinfectants and antibiotics. One proposed solution is applying polymer coatings to the metal parts of the water system to prevent biofilms from forming. Two types of polyampholyte polymers with previously demonstrated nonfouling properties were sent to the ISS in 2021 to test their viability for preventing microbial adhesion in space. However, the only microbial assays performed were microscopy. To enhance this ongoing research project, I developed procedures for culturing, applying, and quantifying Ralstonia pickettii on these polymers. R. pickettii was chosen because it is one of the most prevalent microbes found in the ISS water treatment system. Optical density data was recorded to obtain a growth curve demonstrating a doubling time between 2.83 and 4.88 hours in 30°C, not shaken conditions. Optical density was also correlated to colony forming units in a plating experiment. Another result was design (and pilot testing) of a surface colonization experiment. These results provided vital knowledge about R. pickettii, which will be used for a 2023 payload of antimicrobial polymer coatings on stainless steel, and improved methods for biofilm analysis upon its return to evaluate the efficacy of the coatings.

microbiology↗

NASA NTRS1974

Debond propagation in composite reinforced metals

Strain energy release rates were used to correlate cyclic debonding between metal sheets and composite reinforcement. An expression for the strain energy release rate was derived and applied to fatigue test results for three material systems: graphite bonded to aluminum with both a room temperature and an elevated temperature curing adhesive, and S-glass bonded to aluminum with an elevated temperature curing adhesive. For each material system, several thicknesses were tested with a range of fatigue loads. Cyclic debonding was monitored using a photoelastic technique. A close correlation was found between the observed debond rates and the calculated strain energy release rates for each material system.

Roderick, G. L.↗

NASA NTRS1988

Improving the fatigue resistance of adhesive joints in laminated wood structures

The premature fatigue failure of a laminated wood/epoxy test beam containing a cross section finger joint was the subject of a multi-disciplinary investigation. The primary objectives were to identify the failure mechanisms which occurred during the finger joint test and to provide avenues for general improvements in the design and fabrication of adhesive joints in laminated wood structures.

Laufenberg, Theodore L.↗

NASA NTRS1991

Evaluation of Surlyn 8920 as PHE Visor Material and Evaluations of New Adhesives for Improving Bonding Between Teflon and Stainless Steel at Cryogenic Temperature

Two studies are presented, and in the first study, Surlyn 8920 (an ionic and amorphous low density polyethylene made by Dupont) was evaluated as a possible replacement of Plexyglass G as PHE visor material. Four formulations of the polymer were made by adding different amounts of UV stabilizer, energy quencher, and antioxident in a Brabender Plasticorder. The formulated polymers were molded in the form of sheets in a compression molder. Cut samples from the molded sheets were exposed in a weatherometer and tested on Instron Tensile Tester for strength and elongation. Specially molded samples of the formulated polymers were subjected to Charpy Impact Tests. In the second study, preliminary evaluations of adhesives for improvement of bonding between Teflon and stainless steel (SS) were performed. Kapton, a high temperature polyimide made by Dupont, and a rubber based adhesive made by Potter Paint Co., were evaluated against industrial quality epoxy, the current material used to bond Teflon and SS. The degreased surfaces of the SS discs were etched mechanically, with a few of these etched chemically. The surfaces of the SS discs were etched mechanically, with a few of these etched chemically. Bonding strengths were evaluated using lap shear tests on the Instron Tensile Tester for the samples bonded by Kapton and industrial quality epoxy. Bond strengths were also evaluated using a pull test on the Instron for the samples bonded by Potter adhesive (CWL-152) and industrial quality epoxy. Based on limited lap shear data, Kapton gave bond strength favorable compared to that of industrial epoxy. Based on limited pull test data, Kapton bonded and CWL-152 bonded samples showed poor strength compared to epoxy bonded sample.

Ray, Asit K.↗

NASA NTRS2010

Full-Scale System for Quantifying Loads and Leak Rates of Seals for Space Applications

NASA is developing advanced space-rated vacuum seals in support of future space exploration missions to low-Earth orbit and other destinations. These seals may be 50 to 60 in. (127 to 152 cm) in diameter and must exhibit extremely low leak rates to ensure that astronauts have sufficient breathable air for extended missions to the International Space Station or the Moon. Seal compression loads must be below prescribed limits so as not to overload the mechanisms that compress them during docking or mating, and seal adhesion forces must be low to allow two mated systems to separate when required. NASA Glenn Research Center has developed a new test apparatus to measure leak rates and compression and adhesion loads of candidate full-scale seals under simulated thermal, vacuum, and engagement conditions. Tests can be performed in seal-on-seal or seal-on-flange configurations at temperatures from -76 to 140 F (-60 to 60 C) under operational pressure gradients. Nominal and off-nominal mating conditions (e.g., incomplete seal compression) can also be simulated. This paper describes the main design features of the test apparatus as well as techniques used to overcome some of the design challenges.

Dunlap, Patrick H., Jr.↗

NASA NTRS1974

Feasibility study for the development of low temperature curing adhesives

The feasibility of a new approach for the development of stable, easily handled, room temperature (293 K - 311 K) curing adhesives was studied and demonstrated. The work concentrated on a family of unsaturated amide/ester resins. Twelve candidate resins were synthesized and tested for completeness of cure at room temperature, adhesion to aluminum and titanium, shear strength, moisture resistance and heat stability. The three most promising candidate resins were selected and recommended for further development.

Green, H. E.↗

NASA NTRS1985

Evaluation of high temperature structural adhesives for extended service, phase 4

The evaluation of three phenylquinoxaline polymers as high temperature structural adhesives is presented. These included an experimental crisskubjabke oiktner (X-PQ) and two experimental materials (PPQ-2501) and (PPQ-HC). Lap shear, crack extension, and climing drum peel specimens were fabricated from all three polymers, and tested after thermal, combined thermal/humidity, and stressed Skydrol exposure. All three polymers generally performed well as adhesives at initial test temperatures from 219K (-67 F) to 505K (450 F) and after humidity exposure. The 644K (700 F) cured test specimens exhibited superior Skydrol resistance and thermal stability at 505K (450 F) when compared to the 602K (625 F) cured test specimens.

Hendricks, C. L.↗

NASA NTRS2011

Conformal Thin Film Packaging for SiC Sensor Circuits in Harsh Environments

In this investigation sputtered silicon carbide annealed at 300 C for one hour is used as a conformal thin film package. A RF magnetron sputterer was used to deposit 500 nm silicon carbide films on gold metal structures on alumina wafers. To determine the reliability and resistance to immersion in harsh environments, samples were submerged in gold etchant for 24 hours, in BOE for 24 hours, and in an O2 plasma etch for one hour. The adhesion strength of the thin film was measured by a pull test before and after the chemical immersion, which indicated that the film has an adhesion strength better than 10(exp 8) N/m2; this is similar to the adhesion of the gold layer to the alumina wafer. MIM capacitors are used to determine the dielectric constant, which is dependent on the SiC anneal temperature. Finally, to demonstrate that the SiC, conformal, thin film may be used to package RF circuits and sensors, an LC resonator circuit was fabricated and tested with and without the conformal SiC thin film packaging. The results indicate that the SiC coating adds no appreciable degradation to the circuits RF performance. Index Terms Sputter, silicon carbide, MIM capacitors, LC resonators, gold etchants, BOE, O2 plasma

Scardelletti, Maximilian C.↗

NASA NTRS2006

Robust Joining and Integration Technologies for Advanced Metallic, Ceramic, and Composite Systems

Robust integration and assembly technologies are critical for the successful implementation of advanced metallic, ceramic, carbon-carbon, and ceramic matrix composite components in a wide variety of aerospace, space exploration, and ground based systems. Typically, the operating temperature of these components varies from few hundred to few thousand Kelvin with different working times (few minutes to years). The wide ranging system performance requirements necessitate the use of different integration technologies which includes adhesive bonding, low temperature soldering, active metal brazing, diffusion bonding, ARCJoinT, and ultra high temperature joining technologies. In this presentation, a number of joining examples and test results will be provided related to the adhesive bonding and active metal brazing of titanium to C/C composites, diffusion bonding of silicon carbide to silicon carbide using titanium interlayer, titanium and hastelloy brazing to silicon carbide matrix composites, and ARCJoinT joining of SiC ceramics and SiC matrix composites. Various issues in the joining of metal-ceramic systems including thermal expansion mismatch and resulting residual stresses generated during joining will be discussed. In addition, joint design and testing issues for a wide variety of joints will be presented.

Singh, M.↗

NASA NTRS1970

Improvement of adhesive-bonded structural joints

Investigation is described of methods for obtaining uniform shear stress distribution in adhesives used in double-lap bonded joints. Design rules for reducing adhesive peak shear stresses are listed. Test results of an analysis of straight-lap joint design and stepped-lap joint design are given.

Evensen, H. A.↗

NASA NTRS1975

Structural materials research for lighter-than-air systems

Inflatable systems have widespread applications in military, government, and industrial sectors. Improvements in inflatable materials have followed each salient advancement in textiles. The new organic fiber, Kevlar, is a recent and most significant advancement that justified reexamination of old and new inflatable materials' applications. A fertile frontier exists in integrating Kevlar with various other material combinations, in optimization of geometric features, and in selection of thermomechanical characteristics' compatibility with the environment. Expectations regarding Kevlar have been justified by the performance of two experimental materials. Styrene-butadiene-styrene block copolymers appear promising as a constituent adhesive for low temperature applications. Biaxial testing for both strength and material elastic properties is a technology area needing greater awareness and technology growth along with improved facilities. Because of dramatic materials' advancements, inflatable systems appear to be moving toward an increased position in tomorrow's aerospace industry.

Alley, V. L., Jr.↗

NASA NTRS1975

Solid rocket motor nozzles

The steps in the nozzle design process are examined. The nozzle designer's role in defining design requirements and constraints is included along with discussions of each of the three basic phases of the nozzle design process itself: (1) aerodynamic design, in which the gas-contacting surfaces are configured to produce the required performance within the envelope limits; (2) thermal design, in which termal liners and thermal insulators are selected and configured to maintain the surfaces as closely as practical against effects of erosion and to limit the structure temperature to acceptable levels; and (3) structural design, in which materials are selected and configured to support the thermal components and to sustain the predicted loads. Analytical techniques that are used to establish thermal and structural design integrity and to predict nozzle performance are discussed along with methods for nozzle quality assurance. Emphasis is placed on nozzle design and materials for modern high-temperature aluminized propellants. Recurring nozzle design problems of graphite cracking and ejection, differential erosion at material interfaces, lack of sufficient proven nondestructive testing (NDT) techniques, the uncertainty of adhesive bonding, and inadequate definition of material properties, particularly at high temperatures are considered.

Ellis, R. A.↗

NASA NTRS1982

Development of an all-metal thick film cost effective metallization system for solar cells

Electrodes made with pastes produced under the previous contract were analyzed and compared with raw materials. A needle-like structure observed on the electroded solar cell was identified as eutectic copper-silicon, a phase considered to benefit the electrical and metallurgical properties of the contact. Electrodes made from copper fluorocarbon and copper silver fluoride also contained this phase but had poor adhesion. A liquid medium, intended to provide transport during carbon fluoride decomposition was incorporated into the paste resulting in better adhesion. The product survived preliminary environmental tests. A 2 cm by 2 cm solar cell made with fluorocarbon activated copper electrodes and gave 7% AMI efficiency (without AR coating). Both silver fluoride and fluorocarbon screened paste electrodes can be produced for approximately $0.04 per watt.

Ross, B.↗

NASA NTRS1985

Influence of the resin on interlaminar mixed-mode fracture

Both literature review data and new data on toughness behavior of seven matrix and adhesive systems in four types of tests were studied in order to assess the influence of the resin on interlaminar fracture. Mixed mode (i.e., various combinations of opening mode 1, G sub 1, and shearing mode 2; G sub 2) fracture toughness data showed that the mixed mode relationship for failure appears to be linear in terms of G sub 1 and G sub 2. The study further indicates that fracture of brittle resins is controlled by the G sub 1 component, and that fracture of many tough resins is controlled by total strain-energy release rate, G sub T. Regarding the relation of polymer structure and the mixed mode fracture: high mode 1 toughness requires resin dilatation; dilatation is low in unmodified epoxies at room temperature/dry conditions; dilatation is higher in plasticized epoxies, heated epoxies, and in modified epoxies; modification improves mode 2 toughness only slightly compared with mode 1 improvements. Analytical aspects of the cracked lap shear test specimen were explored.

Johnson, W. S.↗