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NASA NTRS2002

Adhesive and Composite Properties of a New Phenylethynyl Terminated Imide

A relatively new phenylethynyl terminated imide oligomer (PETI) from the reaction of 2,3,',4'- biphenyltetracarboxylic dianhydride, 4,4'-oxydianiline and endcapped with 4- phenylethynylphthalic anhydride at a calculated number average molecular weight of 5000 g/mole was evaluated as an adhesive and composite matrix. The asymmetric dianhydride imparts a low melt viscosity to the oligomer and a high glass transition temperature to the cured resin. Preliminary adhesive work with titanium (6Al-4V) adherend gave good room temperature (RT) tensile shear strengths and excellent retention of RT strength at 260 C. Preliminary composite work using unsized IM7 carbon fiber provided moderate to high mechanical properties. The chemistry, mechanical, and physical properties of the new PETI in neat resin, adhesive and composite form are presented.

Thompson, C. M.↗

NASA NTRS2003

Analyses of Failure Mechanisms in Woven Graphite/Polyimide Composites with Medium and High Modulus Graphite Fibers Subjected to In-Plane Shear

The application of the Iosipescu shear test for the room and high temperature failure analyses of the woven graphite/polyimide composites with the medium (T-650) and igh (M40J and M60J) modulus graphite fibers is discussed. The M40J/PMR-II-50 and M60J/PMR-II-50 composites were tested as supplied and after thermal conditioning. The effect of temperature and conditioning on the initiation of intralaminar damage and the shear strength of the composites was established.

Kumosa, M.↗

NASA NTRS2003

Mechanical Behaviour of Woven Graphite/Polyimide Composites with Medium and High Modulus Graphite Fibers Subjected to Biaxial Shear Dominated Loads

A major limitation of woven fiber/polymer matrix composite systems is the inability of these materials to resist intralaminar and interlaminar damage initiation and propagation under shear-dominated biaxial loading conditions. There are numerous shear test methods for woven fabric composites, each with its own advantages and disadvantages. Two techniques, which show much potential, are the Iosipescu shear and +/- 45 deg tensile tests. In this paper, the application of these two tests for the room and high temperature failure analyses of woven graphite/polyimide composites is briefly evaluated. In particular, visco-elastic micro, meso, and macro-stress distributions in a woven eight harness satin (8HS) T650/PMR-15 composite subjected to these two tests are presented and their effect on the failure process of the composite is evaluated. Subsequently, the application of the Iosipescu tests to the failure analysis of woven composites with medium (T650) and high (M40J and M60J) modulus graphite fibers and PMR-15 and PMR-II-50 polyimide resins is discussed. The composites were tested as-supplied and after thermal conditioning. The effect of temperature and thermal conditioning on the initiation of intralaminar damage and the shear strength of the composites was established.

Kumose, M.↗

NASA NTRS1997

Rhenium Rocket Manufacturing Technology

The NASA Lewis Research Center's On-Board Propulsion Branch has a research and technology program to develop high-temperature (2200 C), iridium-coated rhenium rocket chamber materials for radiation-cooled rockets in satellite propulsion systems. Although successful material demonstrations have gained much industry interest, acceptance of the technology has been hindered by a lack of demonstrated joining technologies and a sparse materials property data base. To alleviate these concerns, we fabricated rhenium to C-103 alloy joints by three methods: explosive bonding, diffusion bonding, and brazing. The joints were tested by simulating their incorporation into a structure by welding and by simulating high-temperature operation. Test results show that the shear strength of the joints degrades with welding and elevated temperature operation but that it is adequate for the application. Rhenium is known to form brittle intermetallics with a number of elements, and this phenomena is suspected to cause the strength degradation. Further bonding tests with a tantalum diffusion barrier between the rhenium and C-103 is planned to prevent the formation of brittle intermetallics.

Source record↗

NASA NTRS1997

Alternative Processing Method Leads to Stronger Sapphire-Reinforced Alumina Composites

The development of advanced engines for aerospace applications depends on the availability of strong, tough materials that can withstand increasingly higher temperatures under oxidizing conditions. The need for such materials led to the study of an oxide-based composite composed of an alumina matrix reinforced with zirconia-coated sapphire fibers. Because the nonbrittle behavior of this system depends on the interface and its ability to prevent fiber-to-matrix bonding and reduce interfacial shear stress, the microstructure of the zirconia must be carefully controlled during both coating application and composite processing. When it was both porous and unstabilized, zirconia (which does not react easily with alumina) was found to be the most effective material tested in reducing interfacial shear strength between the fiber and matrix.

Jaskowiak, Martha H.↗

NASA NTRS2006

Development of Bonded Joint Technology for a Rigidizable-Inflatable Deployable Truss

Microwave and Synthetic Aperture Radar antenna systems have been developed as instrument systems using truss structures as their primary support and deployment mechanism for over a decade. NASA Langley Research Center has been investigating fabrication, modular assembly, and deployment methods of lightweight rigidizable/inflatable linear truss structures during that time for large spacecraft systems. The primary goal of the research at Langley Research Center is to advance these existing state-of-the-art joining and deployment concepts to achieve prototype system performance in a relevant space environment. During 2005, the development, fabrication, and testing of a 6.7 meter multi-bay, deployable linear truss was conducted at Langley Research Center to demonstrate functional and precision metrics of a rigidizable/inflatable truss structure. The present paper is intended to summarize aspects of bonded joint technology developed for the 6.7 meter deployable linear truss structure while providing a brief overview of the entire truss fabrication, assembly, and deployment methodology. A description of the basic joint design, surface preparation investigations, and experimental joint testing of component joint test articles will be described. Specifically, the performance of two room temperature adhesives were investigated to obtain qualitative data related to tube folding testing and quantitative data related to tensile shear strength testing. It was determined from the testing that a polyurethane-based adhesive best met the rigidizable/inflatable truss project requirements.

Smeltzer, Stanley S., III↗

NASA NTRS2006

Adhesive Bonding of Titanium to Carbon-Carbon Composites for Heat Rejection Systems

High temperature adhesives with good thermal conductivity, mechanical performance, and long term durability are crucial for the assembly of heat rejection system components for space exploration missions. In the present study, commercially available adhesives were used to bond high conductivity carbon-carbon composites to titanium sheets. Bonded pieces were also exposed to high (530 to 600 Kelvin for 24 hours) and low (liquid nitrogen 77K for 15 minutes) temperatures to evaluate the integrity of the bonds. Results of the microstructural characterization and tensile shear strengths of bonded specimens will be reported. The effect of titanium surface roughness on the interface microstructure will also be discussed.

Cerny, Jennifer↗

NASA NTRS2007

Effects of Different Braze Materials and Composite Substrates on Composite/Ti Joints

An ever increasing number of applications require robust joining technologies of dissimilar materials. In this study, three types of ceramic composites (C-C, C-SiC, and SiC-SiC) were vacuum brazed to commercially pure Ti using the Cusil-ABA (63 Ag - 35.5 Cu - 1.75 Ti) active metal braze alloy. The study also compared composite specimens as-fabricated and after surface grinding/polishing. A butt-strap tensile shear strength test was used to evaluate the joined structures at room temperature, 270 and 500 C. The elevated temperatures represent possible use temperatures for some heat rejection type applications. Joint strength will be discussed in light of braze wetting and spreading properties, composite properties, and test temperature.

Morscher, Gregory N.↗

NASA NTRS1989

Fiber reinforced thermoplastic resin matrix composites

Polyimide polymer composites having a combination of enhanced thermal and mechanical properties even when subjected to service temperatures as high as 700.degree. F. are described. They comprise (a) from 10 to 50 parts by weight of a thermoplastic polyimide resin prepared from 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane and (b) from 90 to 50 parts by weight of continuous reinforcing fibers, the total of (a) and (b) being 100 parts by weight. Composites based on polyimide resin formed from 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane and pyromellitic dianhydride and continuous carbon fibers retained at least about 50% of their room temperature shear strength after exposure to 700.degree. F. for a period of 16 hours in flowing air. Preferably, the thermoplastic polyimide resin is formed in situ in the composite material by thermal imidization of a corresponding amide-acid polymer prepared from 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane. It is also preferred to initially size the continuous reinforcing fibers with up to about one percent by weight of an amide-acid polymer prepared from 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane. In this way imidization at a suitable elevated temperature results in the in-situ formation of a substantially homogeneous thermoplastic matrix of the polyimide resin tightly and intimately bonded to the continuous fibers. The resultant composites tend to have optimum thermo-mechanical properties.

Jones, Robert J.↗

NASA NTRS2006

Processing and Properties of a Phenolic Composite System

Phenolic resin systems generate water as a reaction by-product via condensation reactions during curing at elevated temperatures. In the fabrication of fiber reinforced phenolic resin matrix composites, volatile management is crucial in producing void-free quality laminates. A commercial vacuum-bag moldable phenolic prepreg system was selected for this study. The traditional single-vacuum-bag (SVB) process was unable to manage the volatiles effectively, resulting in inferior voidy laminates. However, a double vacuum bag (DVB) process was shown to afford superior volatile management and consistently yielded void-free quality parts. The DVB process cure cycle (temperature /pressure profiles) for the selected composite system was designed, with the vacuum pressure application point carefully selected, to avoid excessive resin squeeze-outs and achieve the net shape and target resin content in the final consolidated laminate parts. Laminate consolidation quality was characterized by optical photomicrography for the cross sections and measurements of mechanical properties. A 40% increase in short beam shear strength, 30% greater flexural strength, 10% higher tensile and 18% higher compression strengths were obtained in composite laminates fabricated by the DVB process.

Hou, Tan-Hung↗

NASA NTRS2008

Characterization of Brazed Joints of C-C Composite to Cu-clad-Molybdenum

Carbon-carbon composites with either pitch+CVI matrix or resin-derived matrix were joined to copper-clad molybdenum using two active braze alloys, Cusil-ABA (1.75% Ti) and Ticusil (4.5% Ti). The brazed joints revealed good interfacial bonding, preferential precipitation of Ti at the composite/braze interface, and a tendency toward de-lamination in resin-derived C-C composite due to its low inter-laminar shear strength. Extensive braze penetration of the inter-fiber channels in the pitch+CVI C-C composites was observed. The relatively low brazing temperatures (<950 C) precluded melting of the clad layer and restricted the redistribution of alloying elements but led to metallurgically sound composite joints. The Knoop microhardness (HK) distribution across the joint interfaces revealed sharp gradients at the Cu-clad-Mo/braze interface and higher hardness in Ticusil (approx.85-250 HK) than in Cusil-ABA (approx.50-150 HK). These C-C/Cu-clad-Mo joints with relatively low thermal resistance may be promising for thermal management applications.

Singh, M.↗

NASA NTRS2010

Laser Surface Preparation for Adhesive Bonding of Ti-6Al-4V

Adhesively bonded structures are potentially lighter in weight than mechanically fastened ones, but existing surface treatments are often considered unreliable. Two main problems in achieving reproducible and durable adhesive bonds are surface contamination and variability in standard surface preparation techniques. In this work three surface pretreatments were compared: laser etching with and without grit blasting and conventional Pasa-Jell treatment. Ti-6Al-4V surfaces were characterized by contact angle goniometry, optical microscopy, and X-ray photoelectron spectroscopy (XPS). Laser -etching was found to produce clean surfaces with precisely controlled surface topographies and PETI-5 lap shear strengths and durabilities were equivalent to those produced with Pasa-Jell.

Belcher, Marcus A.↗

NASA NTRS2010

Polyimides Based on Asymmetric Dianhydrides (II) (a-BPDA vs a-BTDA) for Resin Transfer Molding (RTM)

A new series of low-melt viscosity imide resins (10-20 poise at 280 C) were formulated from asymmetric 2,3,3',4' -benzophenone dianhydride (a-BTDA) and 4-phenylethynylphthalic endcaps, along with 3,4' -oxydianiline, 3,3' -methylenedianiline and 3,3'- diaminobenzophenone, using a solvent-free melt process. a-BTDA RTM resins exhibited higher glass transition temperatures (Tg's = 330-400 C) compared to those prepared by asymmetric 2,3,3',4' -biphenyl dianhydride, (a-BPDA, Tg's = 320-370 C). These low-melt viscosity imide resins were fabricated into polyimide/T650-35 carbon fiber composites by a RTM process. Composites properties of a-BTDA resins, such as open-hole compression and short-beam shear strength, are compared to those of composites made from a-BPDA based resin at room temperature, 288 C and 315 C. These novel, high temperature RTM imide resins exhibit outstanding properties beyond the performance of conventional RTM resins, such as epoxy and BMI resins which have use-temperatures around 177 C and 232 C for aerospace applications.

Chuang, Kathy C.↗

NASA NTRS2011

Effects of Notch Misalignment and Tip Radius on Displacement Field in V-Notch Rail Shear Test as Determined by Photogrammetry

Evolution of the 3D strain field during ASTM-D-7078 v-notch rail shear tests on 8-ply quasi-isotropic carbon fiber/epoxy laminates was determined by optical photogrammetry using an ARAMIS system. Specimens having non-optimal geometry and minor discrepancies in dimensional tolerances were shown to display non-symmetry and/or stress concentration in the vicinity of the notch relative to a specimen meeting the requirements of the standard, but resulting shear strength and modulus values remained within acceptable bounds of standard deviation. Based on these results, and reported difficulty machining specimens to the required tolerances using available methods, it is suggested that a parametric study combining analytical methods and experiment may provide rationale to increase the tolerances on some specimen dimensions, reducing machining costs, increasing the proportion of acceptable results, and enabling a wider adoption of the test method.

Hill, Charles S.↗

NASA NTRS2005

Reactive Additives for Phenylethynyl-Containing Resins

Phenylethynyl-containing reactive additive (PERA) compounds and mixtures have been found to be useful for improving the processability of oligomers, polymers, co-oligomers, and copolymers that contain phenylethynyl groups. The additives can be incorporated in different forms: A solution of an amide acid or an imide of a PERA can be added to a solution of phenylethynyl-containing oligomer, polymer, co-oligomer, or copolymer; or An imide powder of a PERA can be mixed with a dry powder of a phenylethynyl-containing oligomer, polymer, co-oligomer, or copolymer. The effect of a given PERA on the processability and other properties of the resin system depends on whether the PERA is used in the amide acid or an imide form. With proper formulation, the PERA reduces the melt viscosity of the resin and thereby reduces the processing pressures needed to form the adhesive bonds, consolidate filled or unfilled moldings, or fabricate fiber-reinforced composite laminates. During thermal cure, a PERA reacts with itself as well as with the phenylethynyl-containing host resin and thereby becomes chemically incorporated into the resin system. The effects of the PERA on mechanical properties, relative to those of the host resin, depend on the amount of PERA used. Typically, the incorporation of the PERA results in (1) increases in the glass-transition temperature (Tg), modulus of elasticity, and parameters that characterize behavior under compression, and (2) greater retention of the aforementioned mechanical properties at elevated temperatures without (3) significant reduction of toughness or damage tolerance. Of the formulations tested thus far, the ones found to yield the best overall results were those for which the host resin was the amide acid form of a phenylethynyl-terminated imide (PETI) co-oligomer having a molecular weight of 5,000 g/mole [hence, designated PETI-5] and a PERA denoted as PERA-1. PETI-5 was made from 3,3',4'4'-biphenyltetracarboxylic dianhydride, 3,4'-oxydianiline (3,4'-ODA), 1,3-bis(3-aminophenoxy) benzene (1,3-APB), and 4-phenylethynylphthalic anhydride (PEPA). PERA-1 was made from 3,5-diamino- 4.-phenylethynylbenzophenon and equimolar amounts of phthalic anhydride and PEPA. To make PERA-1 in the imide form, the aforementioned ingredients were processed by refluxing in glacial acetic acid. To make the amide form of PERA-1, the ingredients were reacted in N-methyl-2-pyrrolidinone (NMP) under nitrogen at a temperature of 23 C (see figure). On the basis of the processability and other properties, a blend comprising 20 weight percent of PERA-1 and 80 weight percent PETI-5 was selected for further evaluation. Relative to neat PETI-5, the blend exhibited an increase in Tg; improved processability; and comparable values of shear strength in adhesion to titanium panels, open-hole compressive properties, compression properties after impact, and resistance to microcracking.

Connell, John W.↗

NASA NTRS2010

Granular Flow and Dynamics of Lunar Simulants in Excavating Implements

The exploration of the lunar surface will rely on properly designed excavation equipment for surface preparations and for collection of lunar regolith in In-Situ Resource Utilization (ISRU) processes. Performance efficiency, i.e minimizing loading forces while maximizing material collection, and mass and volume reductions are major design goals. The NASA Glenn Research Center has embarked on an experimental program to determine the flow characteristics and dynamic forces produced by excavation operations using various excavator bucket designs. A new large scale soil bin facility, 2.27 m x 5.94 m x 0.76 m (nominally 8 ft. x 20 ft. x 27 in.) in size, capable of accommodating moderately large test implements was used for the simulations of lunar operations. The soil bin is filled with GRC-3simulant (a mixture of industrial sands and silt with a particle size distribution and the bulk mechanical (shear) strength representative of an average of lunar regolith from different regions) and uses motorized horizontal rails and a vertical actuator to drive the implement through the lunar simulant soil. A six-axis load cell and encoders provide well resolved measurements of the three dimensional forces and torques and motion of the bucket. In addition, simultaneous video allows for the analysis of the flow behavior and structure formation of the regolith during excavation. The data may be useful in anchoring soil mechanic models and to provide engineering data for design consideration.

Agui, Juan H.↗

NASA NTRS2011

Pre-Finishing of SiC for Optical Applications

13 Manufacturing & Prototyping A method is based on two unique processing steps that are both based on deterministic machining processes using a single-point diamond turning (SPDT) machine. In the first step, a high-MRR (material removal rate) process is used to machine the part within several microns of the final geometry. In the second step, a low-MRR process is used to machine the part to near optical quality using a novel ductile regime machining (DRM) process. DRM is a deterministic machining process associated with conditions under high hydrostatic pressures and very small depths of cut. Under such conditions, using high negative-rake angle cutting tools, the high-pressure region near the tool corresponds to a plastic zone, where even a brittle material will behave in a ductile manner. In the high-MRR processing step, the objective is to remove material with a sufficiently high rate such that the process is economical, without inducing large-scale subsurface damage. A laser-assisted machining approach was evaluated whereby a CO2 laser was focused in advance of the cutting tool. While CVD (chemical vapor deposition) SiC was successfully machined with this approach, the cutting forces were substantially higher than cuts at room temperature under the same machining conditions. During the experiments, the expansion of the part and the tool due to the heating was carefully accounted for. The higher cutting forces are most likely due to a small reduction in the shear strength of the material compared with a larger increase in friction forces due to the thermal softening effect. The key advantage is that the hybrid machine approach has the potential to achieve optical quality without the need for a separate optical finishing step. Also, this method is scalable, so one can easily progress from machining 50-mm-diameter samples to the 250-mm-diameter mirror that NASA desires.

Rozzi, Jay↗

NASA NTRS2012

Composite with In Situ Plenums

A document describes a high-performance thermal distribution panel (TDP) concept using high-conductivity (greater than 800 W/mK) macro composite skin with in situ heat pipes. The processing technologies proposed to build such a panel result in a one-piece, inseparable assembly with high conductance in both the X and Y planes. The TDP configuration can also be used to produce panels with high structural stiffness. The one-piece construction of the TDP eliminates the thermal interface between the cooling plenums and the heat spreader base, and obviates the need for bulky mounting flanges and thick heat spreaders used on baseline designs. The conductivity of the TDP can be configured to exceed 800 W/mK with a mass density below 2.5 grams per cubic centimeter. This material can provide efficient conductive heat transfer between the in situ heat plenums, permitting the use of thinner panel thicknesses. The plenums may be used as heat pipes, loop heat pipes, or liquid cooling channels. The panel technology used in the TDP is a macro-composite comprised of aluminum-encapsulated annealed pyrolytic graphite (APG). APG is highly aligned crystalline graphite with an in-plane thermal conductivity of 1,700 W/mK. APG has low shear strength and does not constrain the encapsulating material. The proposed concept has no thermal interfaces between the heat pipes and the spreader plate, further improving the overall conductance of the system. The in situ plenums can also be used for liquid cooling applications. The process can be used to fabricate structural panels by adding a second thin sheet.

Montesano, Mark↗