Characterization of Polyimide Matrix Resins and Prepregs

NASA Technical Reports Server (NTRS)

Maximovich, M. G.; Galeos, R. M.

1985-01-01

Graphite/polyimide composite materials are attractive candidates for a wide range of aerospace applications. They have many of the virtues of graphite/epoxies, i.e., high specific strengths and stiffness, and also outstanding thermal/oxidative stability. Yet they are not widely used in the aerospace industry due to problems of procesability. By their nature, modern addition polyimide (PI) resins and prepregs are more complex than epoxies; the key to processing lies in characterizing and understanding the materials. Chemical and rheological characterizations are carried out on several addition polyimide resins and graphite reinforced prepregs, including those based on PMR-15, LARC 160 (AP 22), LARC 160 (Curithane 103) and V378A. The use of a high range torque transducer with a Rheometrics mechanical spectrometer allows rheological data to be generated on prepreg materials as well as neat resins. The use of prepreg samples instead of neat resins eliminates the need for preimidization of the samples and the data correlates well with processing behavior found in the shop. Rheological characterization of the resins and prepregs finds significant differences not readily detected by conventional chemical characterization techniques.

High-temperature resins

NASA Technical Reports Server (NTRS)

Serafini, T. T.

1982-01-01

The basic chemistry, cure processes, properties, and applications of high temperature resins known as polyimides are surveyed. Condensation aromatic polymides are prepared by reacting aromatic diamines with aromatic dianhydrides, aromatic tetracarboxylic acids, or with dialkyl esters of aromatic tetracarboxylic acids, depending on the intended end use. The first is for coatings or films while the latter two are more suitable for polyimide matrix resins. Prepreg solutions are made by dissolving reactants in an aprotic solvent, and advances in the addition of a diamine on the double bond and radical polymerization of the double bond are noted to have yielded a final cure product with void-free characteristics. Attention is given to properties of the Skybond, Pyralin, and NR-150B polyimide prepreg materials and characteristics of aging in the NP-150 polyimides. Finally, features of the NASA-developed PMR polyimides are reviewed.

Evaluation of polyimide/glass fiber composites for construction of light weight pressure vessels for cryogenic propellants

NASA Technical Reports Server (NTRS)

Petker, I.; Segimoto, M.

1973-01-01

The application of polyimide resin as a matrix for glass filament-wound thin metal-lined pressure vessels was studied over a temperature range of (minus) 320 to 600 F. Keramid 601 polyimide was found to perform quite well over the entire range of temperature. Hoop stress values of 425 ksi were determined at 75 F which is equivalent to epoxy resin in similar structures. At -320 and 600 F, 125 and 80% of this strength was retained. Thermal ageing at 500 F for up to 50 hours was studied with severe reduction in strength, but there is evidence that this reduction could be improved. Another polyimide resin studied was P10PA which was found to have processing characteristics inappropriate for filament-winding. NOL ring tensile and shear data was determined from both resins with S-glass. Pressure vessel design, fabrication and test procedures are described in detail.

A review of processable high temperature resistant addition-type laminating resins

NASA Technical Reports Server (NTRS)

Serafini, T. T.; Delvigs, P.

1973-01-01

An important finding that resulted from research that was conducted to develop improved ablative resins was the discovery of a novel approach to synthesize processable high temperature resistant polymers. Low molecular weight polyimide prepolymers end-capped with norbornene groups were polymerized into thermo-oxidatively stable modified polyimides without the evolution of void producing volatile materials. This paper reviews basic studies that were performed using model compounds to elucidate the polymerization mechanism of the so-called addition-type polyimides. The fabrication and properties of polyimide/graphite fiber composites using A-type polyimide prepolymer as the matrix are described. An alternate method for preparing processable A-type polyimides by means of in situ polymerization of monomeric reactants on the fiber reinforcement is also described. Polyimide/graphite fiber composite performance at elevated temperatures is presented for A-type polyimides.

Siloxane containing addition polyimides. II - Acetylene terminated polyimides

NASA Technical Reports Server (NTRS)

Maudgal, S.; St. Clair, T. L.

1984-01-01

Acetylene terminated polyimide oligomers having a range of molecular weights have been synthesized by reacting bis (gamma-aminopropyl) tetramethyldisiloxane, aminophenylacetylene and 3, 3', 4, 4' benzophenonetetracarboxylic dianhydride in different molar ratios. The prepolymers were isolated and characterized for melt flow and cure properties. They show promise as adhesives for bonding titanium to titanium and as matrix resins for graphite cloth reinforced composites. The most promising system has been blended in varying proportions with Thermid 600, a commercially available acetylene terminated polyimide oligomer, and the mixtures have been tested for application as composite matrix resins.

High-Flow, High-Molecular-Weight, Addition-Curing Polyimides

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.; Vannucci, Raymond D.

1993-01-01

In developed series of high-flow PMR-type polyimide resins, 2, 2'-bis(trifluoromethyl)-4, 4'-diaminobiphenyl (BTDB) substituted for 1, 4-pheylenediamine in PMR-II formulation. Polyimides designated either as PMR-12F when nadic ester (NE) end caps used, or as V-CAP-12F when p-aminostyrene end caps used. High-molecular-weight, addition-curing polyimides based on BTBD and HFDE highly processable high-temperature matrix resins used to make composite materials with excellent retention of properties during long-term exposure to air at 650 degrees F or higher temperature. Furthermore, 12F addition-curing polyimides useful for electronic applications; fluorinated rigid-rod polyimides known to exhibit low thermal expansion coefficients as well as low absorption of moisture.

An in vitro study of the effect of different restorative materials on the reliability of a veneering porcelain.

PubMed

Anderson, Matthew R; Chung, Kwok-Hung; Flinn, Brian D; Raigrodski, Ariel J

2013-12-01

Implant-supported, porcelain veneered restorations experience a greater rate of porcelain fracture than tooth-supported restorations. For completely edentulous patients, one approach to minimizing porcelain fracture is to use acrylic resin in the mandible, although its efficacy is unknown. The purpose of this study was to evaluate the reliability of a veneering porcelain fatigued with different restorative materials in vitro. Fifty-nine veneering porcelain disk specimens were fabricated by layering veneering porcelain on nickel-chromium base metal alloy disks. Four groups of different indenter materials fatigued the porcelain specimens: group WC, tungsten carbide served as a control; group FC, pressed leucite glass ceramic; group NHC, nanohybrid composite resin denture tooth; and group AR, unfilled acrylic resin denture tooth. Porcelain specimens were randomly divided into 4 groups (n=14). A step-stress accelerated life-testing model was used. Use-level probability Weibull plots were generated, and the reliability of each group was estimated for a theoretical completion of 50 000 cycles at 150 N. Nanohybrid composite resin and unfilled acrylic resin denture tooth groups had higher reliability than tungsten carbide and leucite glass ceramic groups. No significant differences existed between the reliability of the tungsten carbide and leucite glass ceramic groups and the nanohybrid composite resin and acrylic resin denture tooth groups. Veneering porcelain disk specimens fatigued with the unfilled acrylic resin and nanohybrid composite resin denture tooth indenters exhibited higher reliability than the specimens fatigued with either the tungsten carbide or leucite glass ceramic indenters. All of the veneering porcelain disk specimens failed with the same mode of fracture, although the surface posttest exhibited different fracture characteristics among specimens fatigued with the 4 different materials. Copyright © 2013 Editorial Council for the Journal of Prosthetic Dentistry. Published by Mosby, Inc. All rights reserved.

Resin char oxidation retardant for composites

NASA Technical Reports Server (NTRS)

Bowles, K. J.; Gluyas, R. E.

1981-01-01

Boron powder stabilizes char, so burned substances are shiny, smooth, and free of loose graphite fibers. Resin weight loss of laminates during burning in air is identical for the first three minutes for unfilled and boron-filled samples, then boron samples stabilize.

Fiber reinforced thermoplastic resin matrix composites

NASA Technical Reports Server (NTRS)

Jones, Robert J. (Inventor); Chang, Glenn E. C. (Inventor)

1989-01-01

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.

Statistical Design in Isothermal Aging of Polyimide Resins

NASA Technical Reports Server (NTRS)

Sutter, James K.; Jobe, Marcus; Crane, Elizabeth A.

1995-01-01

Recent developments in research on polyimides for high temperature applications have led to the synthesis of many new polymers. Among the criteria that determines their thermal oxidative stability, isothermal aging is one of the most important. Isothermal aging studies require that many experimental factors are controlled to provide accurate results. In this article we describe a statistical plan that compares the isothermal stability of several polyimide resins, while minimizing the variations inherent in high-temperature aging studies.

Ceramic to metal attachment system. [Ceramic electrode to metal conductor in MHD generator

DOEpatents

Marchant, D.D.

1983-06-10

A composition and method are described for attaching a ceramic electrode to a metal conductor. A layer of randomly interlocked metal fibers saturated with polyimide resin is sandwiched between the ceramic electrode and the metal conductor. The polyimide resin is then polymerized providing bonding.

Develop and demonstrate manufacturing processes for fabricating graphite filament reinforced polymide (Gr/PI) composite structural elements

NASA Technical Reports Server (NTRS)

Chase, V. A.; Harrison, E. S.

1985-01-01

A study was conducted to assess the merits of using graphite/polyimide, NR-150B2 resin, for structural applications on advanced space launch vehicles. The program was divided into two phases: (1) Fabrication Process Development; and (2) Demonstration Components. The first phase of the program involved the selection of a graphite fiber, quality assurance of the NR-150B2 polyimide resin, and the quality assurance of the graphite/polyimide prepreg. In the second phase of the program, a limited number of components were fabricated before the NR-150B2 resin system was removed from the market by the supplier, Du Pont. The advancement of the NR-150B2 polyimide resin binder was found to vary significantly based on previous time and temperature history during the prepregging operation. Strength retention at 316C (600F) was found to be 50% that of room temperature strength. However, the composite would retain its initial strength after 200 hours exposure at 316C (600F). Basic chemistry studies are required for determining NR-150B2 resin binder quality assurance parameters. Graphite fibers are available that can withstand high temperature cure and postcure cycles.

Cyclopentadiene evolution during pyrolysis-gas chromatography of PMR polyimides

NASA Technical Reports Server (NTRS)

Alston, William B.; Gluyas, Richard E.; Snyder, William J.

1992-01-01

The effect of formulated molecular weight (FMW), extent of cure, and cumulative aging on the amount of cyclopentadiene (CPD) evolved from Polymerization of Monomeric Reactants (PMR) polyimides were investigated by pyrolysis-gas chromotography (PY-GC). The PMR polyimides are additional crosslinked resins formed from an aromatic diamine, a diester of an aromatic tetracarboxylic acid and a monoester of 5-norbornene-2, 3-dicarboxylic acid. The PY-GC results were related to the degree of crosslinking and to the thermo-oxidative stability (weight loss) of PMR polyimides. Thus, PY-GC has shown to be a valid technique for the characterization of PMR polyimide resins and composites via correlation of the CPD evolved versus the thermal history of the PMR sample.

All-aromatic biphenylene end-capped polyquinoline and polyimide matrix resins

NASA Technical Reports Server (NTRS)

Droske, J. P.; Stille, J. K.; Alston, W. B.

1985-01-01

Biphenylene end-capped polyquinoline and polyimide resins afford low void content graphite-reinforced composites with good initial properties. However, with both resins, rapid degradation occurs during oxidative isothermal aging at elevated temperatures. The degradation is not observed during isothermal aging under a nitrogen atmosphere which suggests that the biphenylene end-cap (or the resulting crosslink/chain extension structures) is not particularly thermooxidatively stable. The nature of the thermooxidative instability is currently under investigation.

Correlations of norbornenyl crosslinked polyimide resin structures with resin thermo-oxidative stability, resin glass transition temperature and composite initial mechanical properties

NASA Technical Reports Server (NTRS)

Alston, William B.

1988-01-01

PMR (polymerization of monomeric reactants) methodology was used to prepare 70 different polyimide oligomeric resins and 30 different unidirectional graphite fiber/polyimide composites. Monomeric composition as well as chain length between sites of crosslinks were varied to examine their effects on resin thermo-oxidative stability and glass transition temperature (Tg) of the cured/postcured resins. A linear correlation of decreasing 316 C resin weight loss/surface area versus (1) decreasing aliphatic content, or (2) increasing benzylic/aliphatic content stoichiometry ratio over a wide range of resin compositions was observed. An almost linear correlation of Tg versus molecular distance between the crosslinks was also observed. An attempt was made to correlate Tg with initial composite mechanical properties (flexural strength and interlaminar shear strength). However, the scatter in mechanical strength data prevented obtaining a clear correlation. Instead, only a range of composite mechanical properties was obtained at 25, 288, and 316 C. Perhaps more importantly, what did become apparent during the correlation study was (1) the PMR methodology could be used to prepare composites from resins containing a wide variety of monomer modifications, (2) that these composites almost invariably provided satisfactory initial mechanical properties as long as the resins formulated exhibited satisfactory processing flow, and (3) that PMR resins exhibited predictable rates of 316 C weight loss/surface area based on their benzylic/aliphatic stoichiometery ratio.

Process for lowering the dielectric constant of polyimides using diamic acid additives

NASA Technical Reports Server (NTRS)

Stoakley, Diane M. (Inventor); St.clair, Anne K. (Inventor)

1990-01-01

Linear aromatic polyimides with low dielectric constants are produced by adding a diamic acid additive to the polyamic acid resin formed by the condensation of an aromatic dianhydride with an aromatic diamine. The resulting modified polyimide is a better electrical insulator than state-of-the-art commercially available polyimides.

Comparison of the impact of scaler material composition on polished titanium implant abutment surfaces.

PubMed

Hasturk, Hatice; Nguyen, Daniel Huy; Sherzai, Homa; Song, Xiaoping; Soukos, Nikos; Bidlack, Felicitas B; Van Dyke, Thomas E

2013-08-01

The purpose of this study was to compare the impact of the removal of biofilm with hand scalers of different material composition on the surface of implant abutments by assessing the surface topography and residual plaque after scaling using scanning electron microscopy (SEM). Titanium implant analogs from 3 manufacturers (Straumann USA LLC, Andover, Maine, Nobel BioCare USA LLC, Yorba Linda, Cali, Astra Tech Implant Systems, Dentsply, Mölndal, Sweden) were mounted in stone in plastic vials individually with authentic prosthetic abutments. Plaque samples were collected from a healthy volunteer, inoculated into growth medium and incubated with the abutments anaerobically for 1 week. A blinded, calibrated hygienist performed scaling to remove the biofilm using 6 implant scalers (in triplicate), 1 scaler for 1 abutment. The abutments were mounted on an imaging stand and processed for SEM. Images were captured in 3 randomly designated areas of interest on each abutment. Analysis of the implant polished abutment surface and plaque area measurements were performed using ImageJ image analysis software. Surface alterations were characterized by the number, length, depth and the width of the scratches observed. Glass filled resin scalers resulted in significantly more and longer scratches on all 3 abutment types compared to other scalers, while unfilled resin scalers resulted in the least surface change (p < 0.05). Filled resin-graphite reinforced scalers, carbon fiber reinforced resin scalers and titanium scalers resulted in more superficial scratches compared to glass filled resin, as well as more scratches than unfilled resin. No statistically significant differences were found between scalers and abutments with regard to plaque removal. The impact of scalers on implant abutment surfaces varies between abutment types presumably due to different surface characteristics with no apparent advantage of one abutment type over the other with regard to resistance to surface damage. Unfilled resin was found consistently to be the least damaging to abutment surfaces, although all scalers of all compositions caused detectable surface changes to polished surfaces of implant abutments.

Development of lightweight graphite/polyimide sandwich panels, phases 3, 4 and 5

NASA Technical Reports Server (NTRS)

Merlette, J. B.

1972-01-01

Work performed in the last three phases of the program included: (1) face sheet processing; (2) honeycomb core manufacture; (3) face sheet-to-core bonding development; and (4) sandwich panel fabrication and testing. Resin cure studies were a major portion of this effort since processing problems traced to the polyimide matrix resin had to be resolved before quality core and face sheets could be fabricated. Honeycomb core fabrication and testing were conducted by Hexcel Corporation. A total of four graphite/polyimide resin composite cores were fabricated, tested, and reported. Two sandwich panels weighing .48 and .58 lb/sq ft, respectively were designed and fabricated which meet the support structure loads for the shuttle orbiter thermal protection system.

Development of autoclave moldable addition-type polyimides

NASA Technical Reports Server (NTRS)

Vaughan, R. W.; Jones, R. J.; Orell, M. K.; Zakrzewski, G. A.

1976-01-01

Chemistry and processing modifications of the poly(Diels Alder) polyimide (PDA) resin were performed to obtain structural composites suitable for 589 K (600 F) service. This work demonstrated that the PDA resin formulation is suitable for service at 589 K (600 F) for up to 125 hours when used in combination with Hercules HTS graphite fiber. Sandwich panels were autoclave molded using PDA/HTS skins and polyimide/glass honeycomb core. Excellent adhesion between honeycomb core and the facing skins was demonstrated. Fabrication ease was demonstrated by autoclave molding three-quarter scale YF-12 wing panels.

Microshear bond strength of composite resins to enamel and porcelain substrates utilizing unfilled versus filled resins.

PubMed

Najafi-Abrandabadi, Ahmad; Najafi-Abrandabadi, Siamak; Ghasemi, Amir; Kotick, Philip G

2014-11-01

Failures such as marginal discoloration and composite chipping are still the problems of tooth-colored restorations on the substrate of enamel and porcelain, which some of these problems are consequently as a result of failures in the bonding layer. Using filled resin has been recently introduced to increase the bond strength of this layer. The aim of this study was to compare the microshear bond strength (μ-SBS) of composite resins to enamel incubated in periods of 24 h and 9 months and porcelain with unfilled resin and flowable composites (filled resin). In this in vitro study, two groups of 75 enamel samples with different storage times (24 h and 9 months) and a group of 75 porcelain samples were used. They were divided into 5 experimental groups of 15 samples in each. Composite cylinders in tygon tubes were bonded on the surface of acid-etched enamel and pretreated porcelain. Wave, Wave MV, Wave HV, Grandioflow and Margin Bond were used as bonding agents. The μ-SBS was measured at the speed of 1.0 mm/min. The bond strengths were analyzed with one-way analysis of variance (ANOVA) test followed by Tukey test. P < 0.05 was selected as the level of statistical significance in this study. The results showed that for enamel (24 h), the μ-SBS of the Wave MV and Wave HV groups were significantly lower than the Margin Bond group. Tukey test indicated the absence of a significant difference between the μ-SBS of the Wave group and the Margin Bond group. However, the μ-SBS of the Grandioflow group was significantly higher than the one for the Margin Bond as a bonding agent. In enamel (9 months), there was a significant difference between the Grandioflow and Margin Bond groups. Regarding bonding to the porcelain the one-way ANOVA test did not show a significant difference among the groups. This study revealed that flowable composites (filled resins) can be used instead of unfilled resins in bonding composite resins to enamel and porcelain substrates.

Advanced thermoplastic resins, phase 1

NASA Technical Reports Server (NTRS)

Hendricks, C. L.; Hill, S. G.; Falcone, A.; Gerken, N. T.

1991-01-01

Eight thermoplastic polyimide resin systems were evaluated as composite matrix materials. Two resins were selected for more extensive mechanical testing and both were versions of LaRC-TPI (Langley Research Center - Thermoplastic Polyimide). One resin was made with LaRC-TPI and contained 2 weight percent of a di(amic acid) dopant as a melt flow aid. The second system was a 1:1 slurry of semicrystalline LaRC-TPI powder in a polyimidesulfone resin diglyme solution. The LaRC-TPI powder melts during processing and increases the melt flow of the resin. Testing included dynamic mechanical analysis, tension and compression testing, and compression-after-impact testing. The test results demonstrated that the LaRC-TPI resins have very good properties compared to other thermoplastics, and that they are promising matrix materials for advanced composite structures.

Solventless LARC-160 Polyimide Matrix Resin. [applied for use in aerospace engineering

NASA Technical Reports Server (NTRS)

Stclair, T. L.; Jewell, R. A.

1978-01-01

The addition polyimide, LARC-160, which was originally synthesized from low cost liquid monomers as a laminating resin in ethanol, was prepared as a solventless, high viscosity, neat liquid resin. The resin was processed by hot-melt coating techniques into graphite prepreg with excellent tack and drape. Comparable data on graphite reinforced laminates made from solvent-coated and various hot-melt coated prepreg were generated. LARC-160, because of its liquid nature, can be easily autoclave processed to produce low void laminates. Liquid chromatographic fingerprints indicate good reaction control on resin scale ups. Minor changes in monomer ratios were also made to improve the thermal aging performance of graphite laminates.

Thermo-elastic nondestructive evaluation of fatigue damage in PMR-15 resin

NASA Astrophysics Data System (ADS)

Welter, J. T.; Sathish, S.; Tandon, G. P.; Schehl, N.; Cherry, M.; Nalladega, V.; Lindgren, E. A.; Hall, R.

2012-05-01

Thermoset polyimide resins are used as the polymer matrix in high temperature composites for aerospace applications such as engine shrouds. At these locations the components have to withstand high temperatures and significant vibration. A number of studies have investigated the effects of thermal exposure on mechanical properties of polyimide resins, and the effects of fatigue on thermoplastics have been discussed at length. However, the effects of fatigue on thermosets, in particular polyimides, have largely been overlooked. In this paper we present studies of nondestructive evaluation of fatigue damage in a thermoset polyimide resin, PMR-15, performed by measuring the changes in the evolution of heat in the samples during cyclic loading. The temperature changes are measured using a high sensitivity IR camera as a function of number of fatigue cycles. Interrupted fatigue tests were performed on four samples. The temperature rise during an increment of fatigue cycling shows two linear regions each with a different slope (region 1 and region 2). Region 1 remains constant for every increment of fatigue, while region 2 increases. The onset of region 2 occurs at the same increase in temperature due to hysteretic heating for all samples. Experimental observations are explained using a phenomenological two phase model based on crosslinking density variations in observed in other thermoset resins at microscopic scales. The results of these experiments are discussed in reference to utilizing this technique for detection and evaluation of fatigue in PMR-15 resin and composites.

Influence of excess diamine on properties of PMR polyimide resins and composites

NASA Technical Reports Server (NTRS)

Hurwitz, F. I.

1980-01-01

By varying the stoichiometry of the reactants in the preparation of PMR polyimide resin, changes occur in molecular weight distribution which influence the rheological properties and thus the processability of the resin, as well as the mechanical properties of the composite. The influence of 1-10 percent molar excess MDA on the molecular weight distribution and rheological properties of an imidized PMR system were exposed. Molecular weight distribution is characterized by gel permeation chromatography of the imidized molding compound; shear viscosity is related to changes in average molecular weight. The thermo-oxidative stability at 600 F, glass transition temperature, flexural and interlaminar shear properties of PMR polyimide/Celion 6000 graphite fiber composites are compared as a function of the percent excess MDA in the monomer reactant mixture.

The effect of diamic acid additives on the dielectric constant of polyimides

NASA Technical Reports Server (NTRS)

Stoakley, Diane M.; St. Clair, Anne K.

1988-01-01

The effect of six selected diamic acids additives (including 2,2-prime bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride-aniline (An); 4,4-prime-oxydiphthalic anhydride-An, 3,3-prime diaminodiphenyl sulfone-phthalic anhydride (PA); 4,4-prime-oxydianiline-PA; 2,2-bis 4(4-aminophenoxy)phenyl hexafluoropropane-PA; and 2,2-bis 4(3-aminophenoxy)phenyl hexafluoropropane-PA) on the dielectric constants of low-dielectric-constant polyimide resins was evaluated. It was found that the effect of the incorporation of the diamic acids on reducing the dielectric constant of polyimides may be limited as the dielectric constant of the base resin itself becomes very low. The additives were found to lower the resin's values of glass transition temperature, with no effect on thermooxidative stability.

Polyimide Composites from 'Salt-Like' Solution Precursors

NASA Technical Reports Server (NTRS)

Cano, Roberto J.; Hou, Tan H.; Weiser, Erik S.; SaintClair, Terry L.

2001-01-01

Four NASA Langley-developed polyimide matrix resins, LaRC(TM)-IA, LaRC(TM)-IAX, LaRC(TM)-8515 and LaRC(TM)-PETI-5, were produced via a 'saltlike' process developed by Unitika Ltd. The salt-like solutions (65% solids in NMP) were prepregged onto Hexcel IM7 carbon fiber using the NASA LaRC multipurpose tape machine. Process parameters were determined and composite panels fabricated. The temperature dependent volatile depletion rates, the thermal crystallization behavior and the resin rheology were characterized. Composite molding cycles were developed which consistently yielded well consolidated, void-free laminated parts. Composite mechanical properties such as the short beam shear strength; the longitudinal and transverse flexural strength and flexural modulus; the longitudinal compression strength and modulus; and the open hole compression strength and compression after impact strength were measured at room temperature and elevated temperatures. The processing characteristics and the composite mechanical properties of the four intermediate modulus carbon fiber/polyimide matrix composites were compared to existing data on the same polyimide resin systems and IM7 carbon fiber manufactured via poly(amide acid) solutions (30-35% solids in NMP). This work studies the effects of varying the synthetic route on the processing and mechanical properties of the polyimide composites.

Polyimide composites: Application histories

NASA Technical Reports Server (NTRS)

Poveromo, L. M.

1985-01-01

Advanced composite hardware exposed to thermal environments above 127 C (260 F) must be fabricated from materials having resin matrices whose thermal/moisture resistance is superior to that of conventional epoxy-matrix systems. A family of polyimide resins has evolved in the last 10 years that exhibits the thermal-oxidative stability required for high-temperature technology applications. The weight and structural benefits for organic-matrix composites can now be extended by designers and materials engineers to include structures exposed to 316 F (600 F). Polyimide composite materials are now commercially available that can replace metallic or epoxy composite structures in a wide range of aerospace applications.

Development of design data for graphite reinforced epoxy and polyimide composites

NASA Technical Reports Server (NTRS)

Scheck, W. G.

1974-01-01

Processing techniques and design data were characterized for a graphite/epoxy composite system that is useful from 75 K to 450 K, and a graphite/polyimide composite system that is useful from 75 K to 589 K. The Monsanto 710 polyimide resin was selected as the resin to be characterized and used with the graphite fiber reinforcement. Material was purchased using the prepreg specification for the design data generation for both the HT-S/710 and HM-S/710 graphite/polyimide composite system. Lamina and laminate properties were determined at 75 K, 297 K, and 589 K. The test results obtained on the skin-stringer components proved that graphite/polyimide composites can be reliably designed and analyzed much like graphite/epoxy composites. The design data generated in the program includes the standard static mechanical properties, biaxial strain data, creep, fatigue, aging, and thick laminate data.

Prototype rigid polyimide components. [application of Apollo technology to commercial nonflammable materials

NASA Technical Reports Server (NTRS)

Wykes, D. H.

1975-01-01

The activity is reported which was conducted for utilizing spin-off Apollo base technology to fabricate a variety of commercial and aerospace related parts that are nonflammable and resistant to high-temperature degradation. Manufacturing techniques and the tooling used to fabricate each of the polyimide/glass structures is discussed. A brief history, tracing the development of high-temperature polyimide resins, is presented along with a discussion of the properties of DuPont's PI 2501/glass material (later redesignated PI 4701/glass). Mechanical and flammability properties of DuPont's PI 2501/glass laminates are compared with epoxy, phenolic, and silicone high-temperature resin/glass material systems. Offgassing characteristics are also presented. A discussion is included of the current developments in polyimide materials technology and the potential civilian and government applications of polyimide materials to reduce fire hazards and increase the survivability of men and equipment.

High-temperature adhesives for bonding polyimide film. [bonding Kapton film for solar sails

NASA Technical Reports Server (NTRS)

St.clair, A. K.; Slemp, W. S.; St.clair, T. L.

1980-01-01

Experimental polyimide resins were developed and evaluated as potential high temperature adhesives for bonding Kapton polyimide film. Lap shear strengths of Kapton/Kapton bonds were obtained as a function of test temperature, adherend thickness, and long term aging at 575 K (575 F) in vacuum. Glass transition temperatures of the polyimide/"Kapton" bondlines were monitored by thermomechanical analysis.

Transfer molding of PMR-15 polyimide resin

NASA Technical Reports Server (NTRS)

Reardon, J. P.; Moyer, D. W.; Nowak, B. E.

1985-01-01

Transfer molding is an economically viable method of producing small shapes of PMR-15 polyimide. It is shown that with regard to flexural, compressive, and tribological properties transfer-molded PMR-15 polyimide is essentially equivalent to PMR-15 polyimide produced by the more common method of compression molding. Minor variations in anisotropy are predictable effects of molding design and secondary finishing operations.

Tough high performance composite matrix

NASA Technical Reports Server (NTRS)

Pater, Ruth H. (Inventor); Johnston, Norman J. (Inventor)

1994-01-01

This invention is a semi-interpentrating polymer network which includes a high performance thermosetting polyimide having a nadic end group acting as a crosslinking site and a high performance linear thermoplastic polyimide. Provided is an improved high temperature matrix resin which is capable of performing in the 200 to 300 C range. This resin has significantly improved toughness and microcracking resistance, excellent processability, mechanical performance, and moisture and solvent resistances.

Improved high-temperature resistant matrix resins

NASA Technical Reports Server (NTRS)

Green, H. E.; Chang, G. E.; Wright, W. F.; Ueda, K.; Orell, M. K.

1989-01-01

A study was performed with the objective of developing matrix resins that exhibit improved thermo-oxidative stability over state-of-the-art high temperature resins for use at temperatures up to 644 K (700 F) and air pressures up to 0.7 MPa (100 psia). The work was based upon a TRW discovered family of polyimides currently licensed to and marketed by Ethyl Corporation as EYMYD(R) resins. The approach investigated to provide improved thermo-oxidative properties was to use halogenated derivatives of the diamine, 2, 2-bis (4-(4-aminophenoxy)phenyl) hexafluoropropane (4-BDAF). Polyimide neat resins and Celion(R) 12,000 composites prepared from fluorine substituted 4-BDAF demonstrated unexpectedly lower glass transition temperatures (Tg) and thermo-oxidative stabilities than the baseline 4-BDAF/PMDA polymer.

A tough high performance composite matrix

NASA Technical Reports Server (NTRS)

Pater, Ruth H. (Inventor); Johnston, Norman J. (Inventor)

1992-01-01

This invention is a semi-interpenetrating polymer network which includes a high performance thermosetting polyimide having a nadic end group acting as a crosslinking site and a high performance linear thermoplastic polyimide. An improved high temperature matrix resin is provided which is capable of performing in the 200 to 300 C range. This resin has significantly improved toughness and microcracking resistance, excellent processability, mechanical performance and moisture and solvent resistances.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Driscoll, S.B.; Walton, T.C.

Polyimides have gained wide acceptance for use in many aerospace composite, electrical, and industrial applications. The intent of this work is to share with the reader practical knowledge of how some of the currently available commercial systems perform. Several prepreg processable polyimide systems were evaluated for adhesive properties and characterized with the use of SEM, TGA, DSC, TMA, Dynamic Spectroscopy, and Force vs. Time Electronic Impact Analyses for comparison. The chemistry and nature of these resin systems is reviewed, including several BMIs (new hot melts examined)., Amide-Imides (Al) and Thermoplastic Polyimide (TPI). PMR-15 and a high temperature epoxy resin aremore » included for comparison of high temperature properties. 17 references.« less

Replacement of MDA with more oxidatively stable diamines in PMR-polyimides

NASA Technical Reports Server (NTRS)

Alston, W. B.

1985-01-01

Studies are performed to investigate the effect of substituting 4,4'-oxydianiline and 1,1-bis(4-aminophenyl)-1-phenyl-2,2,2-trifluoroethane for the 4,4'-methylenedianiline in PMR polyimide matrix resin. Graphite fiber reinforced composites are fabricated from unsized Celion 6000 and PMR-polyimide matrix resins having formulated molecular weights in the range of 1500 to 2400. The composite processing characteristics are investigated and the initial room temperature and 316 C (600 F) composite mechanical properties are determined. Comparative 316 C composite weight losses and 316 C mechanical properties retention after prolonged 316 C air exposure are also determined.

Processable high temperature resistant addition type polyimide laminating resins

NASA Technical Reports Server (NTRS)

Serafini, T. T.; Delvigs, P.

1973-01-01

Basic studies that were performed using model compounds to elucidate the polymerization mechanism of the so-called addition-type (A-type) polyimides are reviewed. The fabrication and properties of polyimide/graphite fiber composites using A-type polyimide prepolymers as the matrix are also reviewed. An alternate method for preparing processable A-type polyimides by means of in situ polymerization of monomer reactants (PMR) on the fiber reinforcement is described. The elevated temperature properties of A-type PMR/graphite fiber composites are also presented.

Fabrication and characterization of nanoclay modified PMR type polyimide composites reinforced with 3D woven basalt fabric

NASA Astrophysics Data System (ADS)

Xie, Jianfei; Qiu, Yiping

2009-07-01

Nanoclay modified PMR type polyimide composites were prepared from 3D orthogonal woven basalt fiber performs and nanoclay modified polyimide matrix resin, which derived from methylene dianiline (MDA), dimethyl ester of 3,3',4,4'- oxydiphthalic acid (ODPE), monomethyl ester of cis-5-norbornene-endo-2,3-dicarboxylic acid (NE) and nanoclay. The Na+-montmorillonite was organically treated using a 1:1 molar ratio mixture of dodecylamine (C12) and MDA. The rheological properties of neat B-stage PMR polyimide and 2% clay modified B-stage PMR polyimide were investigated. Based on the results obtained from the rheological tests, a two step compression molding process can be established for the composites. In the first step, the 3D fabric preforms were impregnated with polyimide resin in a vacuum oven and heated up for degassing the volatiles and by-products. In the second step, composites were compressed. The internal structure of the composites was observed by a microscope. Incorporation of 2% clay showed an improvement in the Tg and stiffness of the PMR polyimide. The resulting composites exhibited high thermal stability and good mechanical properties.

Processable polyimide adhesive and matrix composite resin

NASA Technical Reports Server (NTRS)

Pratt, J. Richard (Inventor); St.clair, Terry L. (Inventor); Progar, Donald J. (Inventor)

1990-01-01

A high temperature polyimide composition prepared by reacting 4,4'-isophthaloyldiphthalic anhydride with metaphenylenediamine is employed to prepare matrix resins, adhesives, films, coatings, moldings, and laminates, especially those showing enhanced flow with retention of mechanical and adhesive properties. It can be used in the aerospace industry, for example, in joining metals to metals or metals to composite structures. One area of application is in the manufacture of lighter and stronger aircraft and spacecraft structures.

High Temperature VARTM with LaRC Polyimides

NASA Technical Reports Server (NTRS)

Cano, Roberto J.; Grimsley, Brian W.; Jensen, Brian J.; Kellen, Charles B.

2004-01-01

Recent work at NASA Langley Research Center (LaRC) has concentrated on developing new polyimide resin systems for advanced aerospace applications that can be processed without the use of an autoclave. Polyimide composites are very attractive for applications that require a high strength to weight ratio and thermal stability. Vacuum assisted resin transfer molding (VARTM) has shown potential to reduce the manufacturing cost of composite structures. In VARTM, the fibrous preform is infiltrated on a rigid tool surface contained beneath a flexible vacuum bag. Both resin injection and fiber compaction are achieved under pressures of 101.3 KPa or less. Recent studies have demonstrated the feasibility of the VARTM process for fabrication of void free structures utilizing epoxy resin systems with fiber volume fractions approaching 60%. In this work, the VARTM process has been extended to the fabrication of composite panels from polyimide systems developed at the Langley Research Center. This work has focused on processing LARC(trademark) PETI-8 (Langley Research Center Phenylethynyl Terminated Imide- 8), an aromatic polyimide based on 3,3',4,4' -biphenyltetracarboxylic dianhydride, a 50:50 molar ratio of 3,4'-oxydianiline and 1,3-bis(3-aminophenoxy)benzene, with 4-phenylethynylphthalic anhydride as the endcapping agent. Various molecular weight versions were investigated to determine their feasibility of being processed by VARTM at elevated temperatures. An injection temperature of approximately 280 C was required to achieve the necessary viscosity (<5 Poise) for flow at VARTM pressures. Laminate quality and initial mechanical properties are presented for LARC(trademark) PETI-8 and 6k IM7 uniweave fabric.

High Temperature Adhesives for Bonding Kapton

NASA Technical Reports Server (NTRS)

Stclair, A. K.; Slemp, W. S.; Stclair, T. L.

1978-01-01

Experimental polyimide resins were developed and evaluated as potential high temperature adhesives for bonding Kapton polyimide film. Lap shear strengths of Kapton/Kapton bonds were obtained as a function of test temperature, adherend thickness, and long term aging at 575K (575 F) in vacuum. Glass transition temperatures of the polyimide/Kapton bondlines were monitored by thermomechanical analysis.

High temperature adhesives for bonding Kapton

NASA Technical Reports Server (NTRS)

Saint Clair, A. K.; Slemp, W. S.; Saint Clair, T. L.

1978-01-01

Experimental polyimide resins have been developed and evaluated as potential high temperature adhesives for bonding Kapton polyimide film. Lap shear strengths of 'Kapton'/'Kapton' bonds were obtained as a function of test temperature, adherend thickness, and long term aging at 575K (575 F) in vacuum. Glass transition temperatures of the polyimide/'Kapton' bondlines were monitored by thermomechanical analysis.

Burning characteristics and fiber retention of graphite/resin matrix composites

NASA Technical Reports Server (NTRS)

Bowles, K. J.

1980-01-01

Graphite fiber reinforced resin matrix composites were subjected to controlled burning conditions to determine their burning characteristics and fiber retention properties. Two types of burning equipment were used. Small samples were burned with a natural gas fired torch to study the effects of fiber orientation and structural flaws such as holes and slits that were machined into the laminates. Larger laminate samples were burned in a Heat Release Rate Calorimeter. Unidirectional epoxy/graphite and polyimide/graphite composites and boron powder filled samples of each of the two composite systems were burn tested and exposed to a thermal radiation. The effects of fiber orientation, flaws, and boron filler additives to the resins were evaluated. A high char forming polyimide resin was no more effective in retaining graphite fibers than a low char forming epoxy resin when burning in air.

Semi-interpenetrating polymer network for tougher and more microcracking resistant high temperature polymers

NASA Technical Reports Server (NTRS)

Pater, Ruth H. (Inventor)

1992-01-01

This invention is a semi-interpenetrating polymer network which includes a high performance thermosetting polyimide having a nadic end group acting as a crosslinking site and a high performance linear thermoplastic polyimide. An improved high temperature matrix resin is provided which is capable of performing at 316 C in air for several hundreds of hours. This resin has significantly improved toughness and microcracking resistance, excellent processability and mechanical performance, and cost effectiveness.

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

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.; Criss, Jim M.; Mintz, Eric A.

2010-01-01

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.

Viscoelastic properties of addition-cured polyimides used in high temperature polymer matrix composites

NASA Technical Reports Server (NTRS)

Roberts, Gary D.; Malarik, Diane C.; Robaidek, Jerrold O.

1991-01-01

The viscoelastic properties of an addition-cured polyimide, PMR-15, were evaluated through dynamic mechanical and stress relaxation testing. Below the glass transition temperature, the dynamic mechanical properties of the composites are strongly affected by the absorbed moisture in the resin. At temperature 20 C and more above the glass transition temperature, the storage modulus increases continuously with time, indicating that additional crosslinking is occurring in the resin. For resin moisture contents less than 2 percent, stress relaxation curves measured at different temperatures can be superimposed using horizontal shifts along the log(time) axis with only small shifts along the vertical axis.

New High Temperature Cross Linking Monomers

NASA Technical Reports Server (NTRS)

Scola, Daniel A.

1978-01-01

This report describes the results of a one-year program designed to synthesize new, nonvolatile crosslinking monomers and to prove their feasibility in the development of lower temperature curing PMR-polyimide resins with high temperature capability. The objective of this program is to develop PMR-polyimide resins capable of being processed at a maximum temperature of 232C to 288C (450F to 500F) without sacrifice of the high temperature 316C (600F) capability of the state-of-the-art PMR-15 polyimide resin. Four monomethyl esters were synthesized and characterized for use in the crosslinking studies. It was found that all four crosslinkers were capable of entering into a crosslinking reaction to produce polymer specimens which were strong, dense and free of voids. The infrared and DSC studies of each crosslinker with monomers 4,4'-methylenedianiline (MDA) and the dimethyl ester of 3,3',4,4'-benzophenonetetracarboxylic acid (BTDE) comprising the resin systems, crosslinker/MDA/BTDE suggested that curing could be accomplished at 288C (550F). However, fabrication of dense, void free polymer specimens required a temperature of 316C (600F) and a pressure of 0.69 MPa (100 psi). The crosslinkers, monomethyl ester of 2,5-bicyclo[2.2.1]heptadiene-2,3-dicarboxylic acid (NDE) and monomethyl ester of maleic acid (MAE) were selected for evaluation in Celion 6000/PMR polyimide composites. These composites were characterized at RT, 288C (550F) and 316C (600F) initially and after isothermal aging at 288C (550F) and 316C (600F) for several hundred hours. The results of the isothermal aging studies suggested that both PMR systems NDE-MDA-BTDE and MAE-MDA-BTDE are promising candidates as matrices for addition type polyimide composites. These studies demonstrated that alternate crosslinkers to NE/MDA/BTDE are feasible, but mechanisms to lower the crosslinking temperature must be developed to provide lower temperature processing PMR-type polyimides.

Polyimide matrix resins for up to 700 deg F service

NASA Technical Reports Server (NTRS)

Jones, R. J.; Chang, G. E.; Powell, S. H.; Green, H. E.

1985-01-01

TRW is in the process of data accumulation that strongly indicates that incorporation of the perfluorsisopropylidene linkage in molecular structures other than those employed in DU Pont's NR-150B polyimides likewise yield polymers demonstrating extremely high thermo-oxidative stability. Polyimide synthetic and characterization studies conducted to date on new polymers incorporating the perfluoroisopropylidene linkage are presented and discussed.

Effects of tetraamine crosslinking agents on the thermomechanical properties of PMR polyimide composites

NASA Technical Reports Server (NTRS)

Delvigs, P.

1976-01-01

The effects were investigated of partial substitution of tetraamine crosslinking agents for diamine reactants on the thermomechanical properties of PMR polyimide resins and graphite fiber-reinforced composites. The effect of tetraamine content on isothermal weight loss, glass transition, and softening temperatures of neat resin samples is discussed. Composites were fabricated using PMR methodology. Monomeric solution of various stoichiometric ratios was used to impregnate Hercules HTS graphite fiber. The mechanical property retention characteristics of the composites at 316 C (600 F) are described.

Determining resin/fiber content of laminates

NASA Technical Reports Server (NTRS)

Garrard, G. G.; Houston, D. W.

1979-01-01

Article discusses procedure where hydrazine is used to extract graphite fibers from cured polyimide resin. Method does not attack graphite fibers and is faster than hot-concentrated-acid digestion process.

Plastic deformation mechanisms in polyimide resins and their semi-interpenetrating networks

NASA Technical Reports Server (NTRS)

Jang, Bor Z.

1990-01-01

High-performance thermoset resins and composites are critical to the future growth of space, aircraft, and defense industries in the USA. However, the processing-structure-property relationships in these materials remain poorly understood. In the present ASEE/NASA Summer Research Program, the plastic deformation modes and toughening mechanisms in single-phase and multiphase thermoset resins were investigated. Both thermoplastic and thermoset polyimide resins and their interpenetrating networks (IPNs and semi-IPNs) were included. The fundamental tendency to undergo strain localization (crazing and shear banding) as opposed to a more diffuse (or homogeneous) deformation in these polymers were evaluated. Other possible toughening mechanisms in multiphase thermoset resins were also examined. The topological features of network chain configuration/conformation and the multiplicity of phase morphology in INPs and semi-IPNs provide unprecedented opportunities for studying the toughening mechanisms in multiphase thermoset polymers and their fiber composites.

Reflective Self-Metallizing Polyimide Films

NASA Technical Reports Server (NTRS)

Thompson, David W. (Inventor); Caplan, Maggie L. (Inventor); St.Clair, Anne (Inventor)

1997-01-01

A silver organic complex, such as silver acetate, is solubilized in a polyamic acid resin or soluble polyimide solution using a suitable solvent such as hexafluoroacetyl acetone. The mixture is stable and can be applied to both flat and contoured surfaces. Application can be performed by casting, dip-coating, spraying, or other suitable techniques. In addition, the mixture can be cast or extruded as a polyimide film which is not applied to an underlying substrate. Upon curing, a flexible silver coated polyimide film is produced.

Electron Paramagnetic Resonance Imaging of the Spatial Distribution of Free Radicals in PMR-15 Polyimide Resins

NASA Technical Reports Server (NTRS)

Ahn, Myong K.; Eaton, Sandra S.; Eaton, Gareth R.; Meador, Mary Ann B.

1997-01-01

Prior studies have shown that free radicals generated by heating polyimides above 300 C are stable at room temperature and are involved in thermo-oxidative degradation in the presence of oxygen gas. Electron paramagnetic resonance imaging (EPRI) is a technique to determine the spatial distribution of free radicals. X-band (9.5 GHz) EPR images of PMR-15 polyimide were obtained with a spatial resolution of approximately 0.18 mm along a 2-mm dimension of the sample. In a polyimide sample that was not thermocycled, the radical distribution was uniform along the 2-mm dimension of the sample. For a polyimide sample that was exposed to thermocycling in air for 300 1-h cycles at 335 C, one-dimensional EPRI showed a higher concentration of free radicals in the surface layers than in the bulk sample. A spectral-spatial two-dimensional image showed that the EPR lineshape of the surface layer remained the same as that of the bulk. These EPRI results suggest that the thermo-oxidative degradation of PMR-15 resin involves free radicals present in the oxygen-rich surface layer.

Electron Paramagnetic Resonance Imaging of the Spatial Distribution of Free Radicals in PMR-15 Polyimide Resins

NASA Technical Reports Server (NTRS)

Ahn, Myong K.; Eaton, Sandra S.; Eaton, Gareth R.; Meador, Mary Ann B.

1997-01-01

Prior studies have shown that free radicals generated by heating polyimides above 300 C are stable at room temperature and are involved in thermo-oxidative degradation in the presence of oxygen gas. Electron Paramagnetic Resonance Imaging (EPRI) is a technique to determine the spatial distribution of free radicals. X-band (9.5 GHz) EPR images of PMR-15 polyimide were obtained with a spatial resolution of about 0.18 mm along a 2 mm dimension of the sample. In a polyimide sample that was not thermocycled, the radical distribution was uniform along the 2 mm dimension of the sample. For a polyimide sample that was exposed to thermocycling in air for 300 one-hour cycles at 335 C, one-dimensional EPRI showed a higher concentration of free radicals in the surface layers than in the bulk sample. A spectral-spatial two-dimensional image showed that the EPR lineshape of the surface layer remained the same as that of the bulk. These EPRI results suggest that the thermo-oxidative degradation of PMR-15 resin involves free radicals present in the oxygen-rich surface layer.

Polyimide Composites Based on Asymmetric Dianhydrides (a-ODPA vs a-BPDA)

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.; Criss, Jim M., Jr.; Mintz, Eric A.

2009-01-01

Two series of low-melt viscosity imide resins (2-15 poise at 260-280 C) were formulated from either asymmetric oxydiphthalic anhydride (a-ODPA) or asymmetric biphenyl dianhydride (a- BPDA) with 4-phenylethynyl endcap (PEPA), along with 3,4'-oxydianiline, 3,4 - methylenedianiline, 3,3 -methylenedianiline or 3,3 -diaminobenzophenone, using a solvent-free melt process. These low-melt viscosity imide resins were fabricated into polyimide/T650-35 carbon fabric composites by resin transfer molding (RTM). Composites from a-ODPA based resins display better open-hole compression strength and short beam shear strength from room temperature to 288 C than that of the corresponding a-BPDA based resins. However, due to the lower Tg s of a-ODPA based resins (265-330 C), their corresponding composites do not possess 315 C use capability while the a-BPDA based composites do. In essence, RTM 370 (T g = 370 C), derived from a-BPDA and 3,4 -ODA and PEPA, exhibits the best overall property performance at 315 C (600 F).

Wet spinning of solid polyamic acid fibers

NASA Technical Reports Server (NTRS)

Dorogy, William E., Jr. (Inventor); Saintclair, Anne K. (Inventor)

1989-01-01

The invention is a process for the production of solid aromatic polyamic acid and polyimide fibers from a wet gel or coagulation bath wet gel using N,N-dimethylacetamide (DMAc) solution of the polyamic acid derived from aromatic dianhydrides such as 3,3',4,4'-benzo phenone tetracarboxylic dianhydride (BTDA) and aromatic diamines such as 4,4'oxydianiline (4,4'-ODA). By utilizing the interrelationship between coagulation medium and concentration, resin inherent viscosity, resin percent solids, filament diameter, and fiber void content, it is possible to make improved polyamic acid fibers. Solid polyimide fibers, obtained by the thermal cyclization of the polyamic acid precursor, have increased tensile properties compared to fibers containing macropores from the same resin system.

Wet spinning of solid polyamic acid fibers

NASA Technical Reports Server (NTRS)

Dorogy, William E., Jr. (Inventor); St.clair, Anne K. (Inventor)

1991-01-01

The invention is a process for the production of solid aromatic polyamic acid and polyimide fibers from a wet gel or coagulation bath wet gel using N,N-dimethylacetamide (DMAc) solutions of the polyamic acid derived from aromatic dianhydrides such as 3,3',4,4' benzophenonetetra carboxylic dianhydride (BTDA) and aromatic diamines such as 4,4'-oxydianiline (4,4'-ODA). By utilizing the relationship among coagulation medium and concentration, resin inherent viscosity, resin percent solids, filament diameter, and fiber void content, it is possible to make improved polyamic acid fibers. Solid polyimide fibers, obtained by the thermal cyclization of the polyamic acid precursor, have increased tensile properties compared to fibers containing macropores from the same resin system.

Structure-to-glass transition temperature relationships in high temperature stable condensation polyimides

NASA Technical Reports Server (NTRS)

Alston, W. B.; Gratz, R. F.

1985-01-01

The presence of a hexafluoroisopropylidene (6F) connecting group in aryl dianhydrides used to prepare aromatic condensation polyimides provides high glass transition temperature (T sub g) polyimides with excellent thermo-oxidative stability. The purpose of this study was to determine if a trifluorophenyl-ethylidene (3F) connecting group would have a similar effect on the T sub g of aromatic condensation polyimides. A new dianhydride containing the 3F connecting group was synthesized. This dianhydride and an aromatic diamine also containing the 3F connecting group were used together and in various combinations with known diamines or known dianhydrides, respectively, to prepare new 3F containing condensation polyimides. Known polyimides, including some with the 6F connecting linkage, were also prepared for comparison purposes. The new 3F containing polymers and the comparison polymers were prepared by condensation polymerization via the traditional amic-acid polymerization method in N,N-dimethylacetamide solvent. The solutions were characterized by determining their inherent viscosities and then were thermally converted into polyimide films under nitrogen atmosphere at 300 to 500 C, usually 350 C. The T sub g's of the films and resin discs were then determined by thermomechanical analysis and were correlated as a function of the final processing temperatures of the films and resin discs. The results showed that similarities existed in the T sub g's depending on the nature of the connecting linkage in the monomers used to prepare the condensation polyimides.

The Influence of Sizings on the Durability of High-Temperature Polymer Composites

NASA Technical Reports Server (NTRS)

Allred, Ronald E.; Wesson, Sheldon P.; Shin, E. Eugene; Inghram, Linda; McCorkle, Linda; Papadopoulos, Demetrios; Wheeler, Donald; Sutter, James K.

2004-01-01

To increase performance and durability of high-temperature composites for potential rocket engine components, it is necessary to optimize wetting and interfacial bonding between high modulus carbon fibers and high-temperature polyimide resins. Sizings commercially supplied on most carbon fibers are not compatible with polyimides. In this study, the chemistry of sizings on two high-modulus carbon fibers (M40J and M60J, Toray) was characterized as was the chemistry of PMR-II-50 fluorinated polyimide resin. The carbon fibers were characterized using single filament wetting, scanning electron microscopy, fourier transform infrared spectroscopy, and x-ray photoelectron spectroscopic measurements. The polyimide matrix resins were coated onto glass filaments for characterization by wetting measurements. Surface energy components were obtained by wetting with nondispersive (methylene iodide), acidic (ethylene glycol), and basic (formamide) probes. A continuous desizing system that uses an environmentally friendly chemical-mechanical process was developed for tow level fiber. Composites were fabricated with fibers containing the manufacturer's sizing, desized, and further treated with a reactive finish. Results of room-temperature tests after thermal aging show that the reactive finish produces a higher strength and more durable interface compared to the manufacturer's sizing. When exposed to moisture blistering tests, however, the better bonded composite displayed a tendency to delaminate, presumably due to trapping of volatiles.

Electrically conductive polyimides containing silver trifluoroacetylacetonate

NASA Technical Reports Server (NTRS)

Rancourt, James D. (Inventor); Stoakley, Diane M. (Inventor); Caplan, Maggie L. (Inventor); St. Clair, Anne K. (Inventor); Taylor, Larry T. (Inventor)

1996-01-01

Polyimides with enhanced electrical conductivity are produced by adding a silver ion-containing additive to the polyamic acid resin formed by the condensation of an aromatic dianhydride with an aromatic diamine. After thermal treatment the resulting polyimides had surface conductivities in the range of 1.7.times.10.sup.-3 4.5 .OMEGA..sup.-1 making them useful in low the electronics industry as flexible, electrically conductive polymeric films and coatings.

Low-Cost, High Glass-Transition Temperature, Thermosetting Polyimide Developed

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.

1999-01-01

PMR-15 polyimide, developed in the mid-1970's at the NASA Lewis Research Center, is recognized as a state-of-the-art high-temperature resin for composite applications in the temperature range of 500 to 550 F (260 to 288 C). PMR-15 offers easy processing and good property retention at a reasonable cost. For these reasons, it is widely used in both military and commercial aircraft engine components. Traditionally, polyimide composites have been designed for long-term use at 500 to 600 F over thousands of hours. However, new applications in reusable launch vehicles (RLV's) require lightweight materials that can perform for short times (tens of hours) at temperatures between 800 and 1000 F (425 and 538 C). Current efforts at Lewis are focused on raising the use temperature of polyimide composites by increasing the glass-transition temperature of the matrix resins. Achieving this dramatic increase in the upper use temperature without sacrificing polymer and composite processability is a major technical challenge.

Fabrication of graphite/polyimide composite structures.

NASA Technical Reports Server (NTRS)

Varlas, M.

1972-01-01

Selection of graphite/polyimide composite as a prime candidate for high-temperature structural applications involving long-duration temperature environments of 400 to 600 F. A variety of complex graphite/polyimide components has been fabricated, using a match-metal die approach developed for making fiber-reinforced resin composites. Parts produced include sections of a missile adapter skin flange, skin frame section, and I-beam and hat-section stringers, as well as unidirectional (0 deg) and plus or minus 45 deg oriented graphite/polyimide tubes in one-, two-, and six-inch diameters.

Structure-to-property relationships in addition cured polymers. 4: Correlations between thermo-oxidative weight losses of norbornenyl cured polyimide resins and their composites

NASA Technical Reports Server (NTRS)

Alston, William B.

1992-01-01

Relationships are identified between the thermo-oxidative stability (TOS) at 316 C of a wide variety of PMR (polymerization of monomeric reactants) addition cured polyimide resins and their corresponding graphite fiber composites. Weight loss results at 316 C confirmed the expected relationship of increasing aliphatic endcap content with decreasing TOS. Moreover, the resin TOS study also showed an unexpected linear correlation of decreasing weight loss to increasing ratio of benzylic diamine to aliphatic endcap in the range of the stoichiometries studied. Only after long term 316 C aging does the dianhydride used with the benzylic diamines become an additional factor in influencing the amount of PMR resin and composite weight losses. Also, the benzylic systems consistently showed much lower resin and composite weight losses at 316 C than the corresponding nonbenzylic norbornenyl resins and composites, except when the nonbenzylic diamine monomer does not contain a connecting group. Instead, this diamine resulted in a 316 C resin and composite weight loss that was only competitive with benzylic type diamines. Results show excellent correlation between TOS of all graphite fiber PMR composites and resins.

Polyimide resins

DOEpatents

Tesoro, Giuliana C.; Sastri, Vinod R.

1993-01-01

A method for the preparation of a polyimide containing reversible crosslinks comprising the step of curing a monomer having the formula ##STR1## wherein R and R' may be the same or different and each is H or lower alkyl having 1-5 carbon atoms under conditions conducive to the formation of a polyimide and thereby forming a polyimide having the formula ##STR2## R and R' are as defined above and n is an integer from 10 to 100. The polyimide may be converted to a soluble polymer by cleaving the disulfide bond in the presence of a solvent and a reducing agent. The reduced polymer may be reformed into the polymer in an oxidation step or into a modified polyimide in other reaction steps. Copolymerization processes are also disclosed.

Optimal Composite Material for Low Cost Fabrication of Large Composite Aerospace Structures using NASA Resins or POSS Nanoparticle Modifications

NASA Technical Reports Server (NTRS)

Lamontia, Mark A.; Gruber, Mark B.; Jensen, Brian J.

2006-01-01

Thermoplastic laminates in situ consolidated via tape or tow placement require full mechanical properties. Realizing full properties requires resin crystallinity to be controlled - partial crystallinity leads to unacceptably low laminate compression properties. There are two approaches: utilize an amorphous matrix resin; or place material made from a semi-crystalline resin featuring kinetics faster than the process. In this paper, a matrix resin evaluation and trade study was completed with commercial and NASA amorphous polyimides on the one hand, and with PEKK mixed with POSS nanoparticles for accelerated crystallinity growth on the other. A new thermoplastic impregnated material, 6 mm wide (0.25-in) AS-4 carbon/LaRC(TradeMark)8515 dry polyimide tow, was fabricated. Since LaRC(TradeMark)8515 is fully amorphous, it attains full properties following in situ consolidation, with no post processing required to build crystallinity. The tow in situ processing was demonstrated via in situ thermoplastic filament winding it into rings.

Study on process and characterization of high-temperature resistance polyimide composite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pan, Ling-Ying; Zhao, Wei-Dong; Liu, Han-Yang

2016-05-18

A novel polyimide composite with upper-use temperature of 420°C was prepared by autoclave process. The thermogravimetic analysis and rheological properties of uncured polyimide resin powders were analyzed. The influences of process parameters and post-treatment process on the properties of composites were also investigated. The morphologies of polyimide composites after shear fracture were observed by scanning electron microscope (SEM). The high-temperature resistance of composite was characterized by dynamic mechanical thermal analyzer (DMTA). Results showed that the imidization reaction mainly occurred in the temperature range of 100°C~220°C, and the largest weight loss rate appearing at 145°C indicated a drastic imidization reaction occurred.more » The melt viscosity of polyimide resin decreased with increasing the temperature between 220°C ∼305°C, and then increased with the increase of temperature due to the molecular crosslinking reactions. The fiber volume contents and void contents could be effectively controlled by applying the pressure step by step. The fiber volume content was sensitive to the initial pressure (P{sub i}) during the imidization. The second-stage pressure (P{sub 2}) and the temperature for applying the P{sub 2} (T{sub 2}) during the imidization had a great effect on the void content of composite. Good mechanical properties and interfacial adhesion of polyimide composite could obtain by optimized process. The post-treatment process can obviously increase the high-temperature resistance of polyimide composite. The polyimide composite treated at 420°C exhibited good retention of mechanical properties at 420°C and had a glass transition temperature (Tg) of 456°C. The retentions of flexible strength, flexible modulus and short beam shear strength of polyimide composite at 420°C were 65%, 84% and 62% respectively.« less

The 3F condensation polyimides: Review and update

NASA Technical Reports Server (NTRS)

Alston, William B.; Gratz, Roy F.

1989-01-01

Nine new condensation polyimides containing the phenyltrifluoroethylidene (3F) linkage were synthesized by the amic-acid route. Several other polyimides, including some with hexafluoroisopropylidene (6F) linkage, were also prepared as controls. Amic-acid solutions were characterized by determining their inherent viscosities prior to thermal conversion into polyimide films. Glass transition temperatures (T sub g), thermogravimetric analysis (TGA), and isothermal weight loss data (at 316, 371, and 371 C under 0.5 MPa air pressure) were obtained for the films. The films were pulverized into molding powders which, in turn, were thermally processed under pressure into neat resin disks. The disks were also characterized by T sub g's and 316 and 371 C isothermal weight losses. The film study identified two new polyimides with T sub g's greater than 371 C and two new polyimides with low rates of weight loss. The resin disks exhibited the same overall trends in T sub g and weight loss as the respective films, however the weight loss per unit surface area was always greater, presumably due to molecular degradation induced during preparation of the molding powders. The overall results indicate that polyimides containing the 3F linkage have T sub g's and thermo-oxidative stability comparable to polyimides containing the 6F group. Alternate technology was also shown by the synthesis of two new polyalkyl substituted 3F diamines and five more new 3F polymers. Their potential as photoresists was demonstrated by T sub g advancement after ultraviolet exposure. Last, four U.S. patents on 3F monomers and polymers were issued and up to eight more are pending.

Studies on Hot-Melt Prepregging on PRM-II-50 Polyimide Resin with Graphite Fibers

NASA Technical Reports Server (NTRS)

Shin, E. Eugene; Sutter, James K.; Juhas, John; Veverka, Adrienne; Klans, Ojars; Inghram, Linda; Scheiman, Dan; Papadopoulos, Demetrios; Zoha, John; Bubnick, Jim

2004-01-01

A second generation PMR (in situ Polymerization of Monomer Reactants) polyimide resin PMR-II-50, has been considered for high temperature and high stiffness space propulsion composites applications for its improved high temperature performance. As part of composite processing optimization, two commercial prepregging methods: solution vs. hot-melt processes were investigated with M40J fabrics from Toray. In a previous study a systematic chemical, physical, thermal and mechanical characterization of these composites indicated the poor resin-fiber interfacial wetting, especially for the hot-melt process, resulted in poor composite quality. In order to improve the interfacial wetting, optimization of the resin viscosity and process variables were attempted in a commercial hot-melt prepregging line. In addition to presenting the results from the prepreg quality optimization trials, the combined effects of the prepregging method and two different composite cure methods, i.e. hot press vs. autoclave on composite quality and properties are discussed.

Studies on Hot-Melt Prepregging of PMR-II-50 Polyimide Resin with Graphite Fibers

NASA Technical Reports Server (NTRS)

Shin, E. Eugene; Sutter, James K.; Juhas, John; Veverka, Adrienne; Klans, Ojars; Inghram, Linda; Scheiman, Dan; Papadopoulos, Demetrios; Zoha, John; Bubnick, Jim

2003-01-01

A Second generation PMR (in situ Polymerization of Monomer Reactants) polyimide resin, PMR-II-50, has been considered for high temperature and high stiffness space propulsion composites applications for its improved high temperature performance. As part of composite processing optimization, two commercial prepregging methods: solution vs. hot-melt processes were investigated with M40J fabrics from Toray. In a previous study a systematic chemical, physical, thermal and mechanical characterization of these composites indicated that poor resin-fiber interfacial wetting, especially for the hot-melt process, resulted in poor composite quality. In order to improve the interfacial wetting, optimization of the resin viscosity and process variables were attempted in a commercial hot-melt prepregging line. In addition to presenting the results from the prepreg quality optimization trials, the combined effects of the prepregging method and two different composite cure methods, i.e., hot press vs. autoclave on composite quality and properties are discussed.

Effects of solvent on solution prepregging of the resin system LaRC{trademark}-IAX-2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cano, R.J.; Massey, C.P.; St. Clair, T.L.

1996-12-31

This work assesses the feasibility of using an alternative solvent for the production of composites from polyimide resin systems via solution prepregging. Previous work on solution prepregging of polyimide systems at NASA Langley Research Center has concentrated on the use of the solvent N-methylpyrrolidinone. An alternative solvent with a similar boiling point, -{gamma}-Butyrolactone, was used to prepare the poly(amide acid) version of LaRC{trademark}-IAX-2. These solutions were subsequently used to prepare prepreg and graphite-reinforced composites. Mechanical properties are presented for the resin system LaRC{trademark}-IAX-2 (4% and 5% offset in stoichiometry and endcapped with phthalic anhydride) impregnated onto Hercules IM7 carbon fiber.more » Results from this work were compared to data obtained on the same resin system which had been solution prepregged with the solvent N-methylpyrrolidinone.« less

Evaluation of inter-laminar shear strength of GFRP composed of bonded glass/polyimide tapes and cyanate-ester/epoxy blended resin for ITER TF coils

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hemmi, T.; Matsui, K.; Koizumi, N.

2014-01-27

The insulation system of the ITER TF coils consists of multi-layer glass/polyimide tapes impregnated a cyanate-ester/epoxy resin. The ITER TF coils are required to withstand an irradiation of 10 MGy from gamma-ray and neutrons since the ITER TF coils is exposed by fast neutron (>0.1 MeV) of 10{sup 22} n/m{sup 2} during the ITER operation. Cyanate-ester/epoxy blended resins and bonded glass/polyimide tapes are developed as insulation materials to realize the required radiation-hardness for the insulation of the ITER TF coils. To evaluate the radiation-hardness of the developed insulation materials, the inter-laminar shear strength (ILSS) of glass-fiber reinforced plastics (GFRP) fabricatedmore » using developed insulation materials is measured as one of most important mechanical properties before/after the irradiation in a fission reactor of JRR-3M. As a result, it is demonstrated that the GFRPs using the developed insulation materials have a sufficient performance to apply for the ITER TF coil insulation.« less

Low-void polyimide resins for autoclave processing

NASA Technical Reports Server (NTRS)

Jones, R. J.; Vaughan, R. W.

1972-01-01

Development of an advanced A-type polyimide, which can be used to produce autoclave molded, low-void content composites suitable for use at temperatures up to 316 C is reported. It consists of a mixture of methyl nadic anhydride, an 80:20 molar ratio of methylene dianaline and thiodianilene, and pyromellitic dianhydride.

Resin/graphite fiber composites

NASA Technical Reports Server (NTRS)

Cavano, P. J.

1974-01-01

Processing techniques were developed for the fabrication of both polyphenylquinoxaline and polyimide composites by the in situ polymerization of monomeric reactants directly on the graphite reinforcing fibers, rather than using previously prepared prepolymer varnishes. Void-free polyphenylquinoxaline composites were fabricated and evaluated for room and elevated flexure and shear properties. The technology of the polyimide system was advanced to the point where the material is ready for commercial exploitation. A reproducible processing cycle free of operator judgment factors was developed for fabrication of void-free composites exhibiting excellent mechanical properties and a long time isothermal life in the range of 288 C to 316 C. The effects of monomer reactant stoichiometry and process modification on resin flow were investigated. Demonstration of the utility and quality of this polyimide system was provided through the successful fabrication and evaluation of four complex high tip speed fan blades.

Prepreg cure monitoring using diffuse reflectance-FTIR. [Fourier Transform Infrared Technique

NASA Technical Reports Server (NTRS)

Young, P. R.; Chang, A. C.

1984-01-01

An in situ diffuse reflectance-Fourier transform infrared technique was developed to determine infrared spectra of graphite fiber prepregs as they were being cured. A bismaleimide, an epoxy, and addition polyimide matrix resin prepregs were studied. An experimental polyimide adhesive was also examined. Samples were positioned on a small heater at the focal point of diffuse reflectance optics and programmed at 15 F/min while FTIR spectra were being scanned, averaged, and stored. An analysis of the resulting spectra provided basic insights into changes in matrix resin molecular structure which accompanied reactions such as imidization and crosslinking. An endo-exothermal isomerization involving reactive end-caps was confirmed for the addition polyimide prepregs. The results of this study contribute to a fundamental understanding of the processing of composites and adhesives. Such understanding will promote the development of more efficient cure cycles.

Oligosilylarylnitrile: The Thermoresistant Thermosetting Resin with High Comprehensive Properties.

PubMed

Wang, Mingcun; Ning, Yi

2018-04-11

One of the highest thermoresistant thermosetting resins ever studied so far, oligosilylarylnitrile resin, was investigated first in this study. Oligosilylarylnitrile was synthesized by lithium-reduced Wurtz-Fittig condensation reaction, and the prepared viscous resin exhibited moderate rheological behaviors while heated purely or together with 20% polysilazane as a cross-linking agent. The thermal curing temperatures were found by differential scanning calorimetry at 268 °C (pure) and 158 °C (with the polysilazane cross-linking agent), which is comparably close to that of polysilylarylacetylene resin (normally at 220-250 °C) but much lower than those of polyimide and phthalonitrile resins (normally >300 °C), indicating the admirable material processability of oligosilylnitrile. The cured oligosilylarylnitrile resins have extremely high thermal resistance, indicated by the results of thermogravimetric analysis (the mass residue at 800 °C is >90% under N 2 ) and dynamic mechanical analysis (the glass-transition temperature is >420 °C). The mechanical property of the oligosilylarylnitrile-matrixed silica-cloth reinforced laminate is comparably close to those of polyimide and phthalonitrile but much higher than that of polysilylarylacetylene, indicating the enviable thermal and mechanical properties of oligosilylnitrile. Thus, among the high-temperature resins ever studied so far, the oligosilylarylnitrile resin was found to have the almost best comprehensive characteristics of processability and properties.

Synthesis and Characterization of a Polyimide-Epoxy Composite for Dental Applications

NASA Astrophysics Data System (ADS)

Yang, An; Xu, Chun

2018-03-01

Epoxy (EP) resins have been employed in dentistry for years, but their intrinsic brittleness demands a reinforcement to make them an ideal dental material that combines strength, toughness, and aesthetics. In this study, an EP resin was reinforced with a low-molecular-weight polyimide (PI). The PI/EP composites were subjected to three-point bending tests and examined by the scanning electron microscopy. It was found that blending PI with EP in proper proportions strengthened EP without sacrificing its toughness. The PI/EP composite could be employed in dentistry as the matrix of fiber-reinforced dental root canal posts.

Development of lightweight graphite/polyimide sandwich panels. Phase 2: Thin gage material manufacture

NASA Technical Reports Server (NTRS)

Merlette, J. B.

1972-01-01

Thin gage materials selected and the rationale for their basic requirements are discussed. The resin used in all prepreg manufacture is Monsanto RS-6234 polyimide. The selected fiber for core manufacture is Hercules HT-S, and the selected fiber for face sheets is Hercules HM-S. The technique for making thin gage prepreg was to wind spread carbon fiber tows into a resin film on a large drum. This technique was found to be superior to others investigated. A total of 22 pounds of 1 to 2 mil/ply prepreg was fabricated for use on the program.

Low-Cost Resin Transfer Molding Process Developed for High-Temperature Polyimide Matrix Composites

NASA Technical Reports Server (NTRS)

1996-01-01

The use of high-temperature polymer matrix composites (PMC's) in aircraft engine applications can significantly reduce engine weight and improve performance and fuel efficiency. High-temperature PMC's, such as those based on the PMR-15 polyimide matrix resin developed by the NASA Lewis Research Center, have been used extensively in military applications where performance improvements have justified their use regardless of the cost involved in producing the component. However, in commercial engines cost is a primary driver, and PMC components must be produced at costs comparable to those of the metal components that they will replace.

Polyphosphazene toughened high performance thermosets

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abu-Shanab, O.L.; Duygulu, M.; Soucek, M.D.

1995-12-31

Two modified polyphosphazenes were synthesized and characterized via FT-IR, {sup 1}H and {sup 31}P NMR, and DSC. Semi-Interpenetrating networks based on phenyl imide substituted polyphosphazene and polyimide thermoset resin designated LaRC{trademark} RP46 were prepared. Grafted copolymers were formed by grafting the backbone of maleimide substituted polyphosphazene into LaRC{trademark} RP46 thermoset resin. Thin films with a 0 to 40 Wt% range of polyphosphazene to polyimide ratio were prepared. A structure-property relationships of these inorganic/organic polymeric matrices were studied and evaluated in terms of fracture toughness, thermo-oxidative stability, thermal, and tensile properties.

Low coefficient of thermal expansion polyimides containing metal ion additives

NASA Technical Reports Server (NTRS)

Stoakley, D. M.; St. Clair, A. K.

1992-01-01

Polyimides have become widely used as high performance polymers as a result of their excellent thermal stability and toughness. However, lowering their coefficient of thermal expansion (CTE) would increase their usefulness for aerospace and electronic applications where dimensional stability is a requirement. The incorporation of metal ion-containing additives into polyimides, resulting in significantly lowered CTE's, has been studied. Various metal ion additives have been added to both polyamic acid resins and soluble polyimide solutions in the concentration range of 4-23 weight percent. The incorporation of these metal ions has resulted in reductions in the CTE's of the control polyimides of 12 percent to over 100 percent depending on the choice of additive and its concentration.

Structure-to-property relationships in addition cured polymers. II - Resin Tg and composite initial mechanical properties of norbornenyl cured polyimide resins

NASA Technical Reports Server (NTRS)

Alston, William B.

1986-01-01

PRM (polymerization of monomeric reactants) methodology was used to prepare thirty different polyimide oligomeric resins. Monomeric composition as well as chain length between sites of crosslinks were varied to examine their effects on glass transition temperature (Tg) of the cured/postcured resins. An almost linear correlation of Tg versus molecular distance between the crosslinks was observed. An attempt was made to correlate Tg with initial mechanical properties (flexural strength and interlaminar shear strength) of unidirectional graphite fiber composites prepared with these resins. However, the scatter in mechanical strength data prevented obtaining as clear a correlation as was observed for the structural modification/crosslink distance versus Tg. Instead, only a range of composite mechanical properties was obtained at the test temperatures studied (room temperature, 288 and 316 C). Perhaps more importantly, what did become apparent during the attempted correlation study was: (1) that PMR methodology could be used to prepare composites from resins that contain a wide variety of monomer modifications, and (2) that these composites almost invariably provided satisfactory initial mechanical properties as long as the resins selected were melt processable.

Structure-to-property Relationships in Addition Cured Polymers 2: Resin Tg Composite Initial Mechanical Properties of Norbornenyl Cured Polyimide Resins

NASA Technical Reports Server (NTRS)

Alston, W. B.

1986-01-01

PRM (polymerization of monomeric reactants) methodology was used to prepare thirty different polyimide oligomeric resins. Monomeric composition as well as chain length between sites of crosslinks were varied to examine their effects on glass transition temperature (Tg) of the cured/postcured resins. An almost linear correlation of Tg versus molecular distance between the crosslinks was observed. An attempt was made to correlate Tg with initial mechanical properties (flexural strength and interlaminar shear strength) of unidirectional graphite fiber composites prepared with these resins. However, the scatter in mechanical strength data prevented obtaining as clear a correlation as was observed for the structural modification/crosslink distance versus Tg. Instead, only a range of composite mechanical properties was obtained at the test temperatures studied (room temperature, 288 and 316 C). Perhaps more importantly, what did become apparent during the attempted correlation study was: (1) that PMR methodology could be used to prepare composites from resins that contain a wide variety of monomer modifications, and (2) that these composites almost invariably provided satisfactory initial mechanical properties as long as the resins selected were melt processable.

Development and fabrication of a graphite polyimide box beam

NASA Technical Reports Server (NTRS)

Nadler, M. A.; Darms, F. J.

1972-01-01

The state-of-the-art of graphite/polyimide structures was evaluated and key design and fabrication issues to be considered in future hardware programs are defined. The fabrication and testing at 500 F of a graphite/polyimide center wing box beam using OV-10A aircraft criteria was accomplished. The baseline design of this box was developed in a series of studies of other advanced composite materials: glass/epoxy, boron/epoxy, and boron/polyimide. The use of this basic design permits ready comparison of the performance of graphite/polyimide with these materials. Modifications to the baseline composite design were made only in those areas effected by the change of materials. Processing studies of graphite fiber polyimide resins systems resulted in the selection of a Modmor II/Gemon L material.

Development of lightweight graphite/polyimide honeycomb. Phase 1: Materials selection

NASA Technical Reports Server (NTRS)

Poesch, J. G.

1971-01-01

The materials selected for the production of extremely lightweight honeycomb sandwich panels are discussed. The resin selected for the first core and face sheet fabrication was Monsanto RS6234 polyimide. The fiber selected for core manufacture was Hercules HT-S, and for face sheets, Hercules HM-S; these selections are discussed.

Recent developments in polyimide and bismaleimide adhesives

NASA Technical Reports Server (NTRS)

Politi, R. E.

1985-01-01

Research on high temperature resin systems has intensified. In the Aerospace Industry, the motivation for this increased activity has been to replace heat resistant alloys of aluminum, stainless steel and titanium by lighter weight glass and carbon fiber reinforced composites. Applications for these structures include: (1) engine nacelles involving long time exposure (thousands of hours) to temperatures in the 150 to 300 C range, (2) supersonic military aircraft involving moderately long exposure (hundreds of hours) to temperatures of 150 to 200 C, and (3) missile applications involving only brief exposure (seconds or minutes) to temperatures up to 500 C and above. Because of fatigue considerations, whenever possible, it is preferable to bond rather than mechanically fasten composite structures. For this reason, the increased usage of high temperature resin matrix systems for composites has necessitated the devlopment of compatible and equally heat stable adhesive systems. The performance of high temperature epoxy, epoxy phenolic and condensation polyimide adhesives is reviewed. This is followed by a discussion of three recently developed types of adhesives: (1) condensation reaction polyimides having improved processing characteristics; (2) addition reaction polyimides; and (3) bismaleimides.

Graphite-fiber-reinforced polyimide liners of various compositions in plain spherical bearings

NASA Technical Reports Server (NTRS)

Sliney, H. E.; Jacobson, T. P.

1978-01-01

A plain spherical bearing design with a ball diameter of 28.6 mm, a race length of 12.7 mm, and a 1.7-mm-thick, molded composite liner was evaluated. The liner material is a self-lubricating composite of graphite-fiber-reinforced polyimide resin (GFRPI). The liner is prepared by transfer molding a mixture of one part chopped graphite fiber and one part partially polymerized resin into the space between the bearing ball and the outer race and then completing the polymerization under heat and pressure. Several liner compositions were evaluated: two types of polyimide, condensation and addition; two types of graphite fiber, low and high modulus; and four powder additives - cadmium oxide, cadmium iodide, graphite fluoride, and molybdenum disulfide. The bearings were oscillated + or - 15 deg at 1 Hz for 20 kilocycles under a radial unit load of 29 MN sq m (4200 psi) in dry air at 25, 200, or 315 C. Both types of fiber and polyimide gave low friction and wear. A simple equation was developed to fit the wear-time data and adequately predicted wear to 100 kilocycles.

LARC-TPI: A multi-purpose thermoplastic polyimide

NASA Technical Reports Server (NTRS)

St.clair, A. K.; St.clair, T. L.

1982-01-01

A linear thermoplastic polyimide, LARC-TPI, was characterized and developed for a variety of high temperature applications. In its fully imidized form, this material can be used as an adhesive for bonding metals such as titanium, aluminum, copper, brass, and stainless steel. LARC-TPI was evaluated as a thermoplastic for bonding large pieces of polyimide film to produce flexible, 100 void-free laminates for flexible circuit applications. The development of LARC-TPI as a potential molding powder, composite matrix resin, high temperature film and fiber is also discussed.

PMR polyimides: Processable high temperature composite matrix resins

NASA Technical Reports Server (NTRS)

Winters, W. E.; Serafini, T. T.

1975-01-01

Processing reproducibility and versatility were demonstrated for producing addition-cured polyimide/graphite fiber composites using an in situ polymerization of monomeric reactants directly on the fiber surface. The polymers so derived, designated PMR polyimides, can be fabricated into composite structures by laminating, random fiber molding or autoclave curing. Composites were determined to be thermally stable and retain useful properties after extended exposures at 550 F to 650 F. The material and fabrication capability were demonstrated by the fabrication and evaluation of prototype complex fan blades.

PMR polyimides - Processable high temperature composite matrix resins

NASA Technical Reports Server (NTRS)

Winters, W. E.; Serafini, T. T.

1975-01-01

Processing reproducibility and versatility were demonstrated for producing addition-cured polyimide/graphite fiber composites using a unique in situ polymerization of monomeric reactants directly on the fiber surface. The polymers so derived, designated PMR polyimides, can be fabricated into composite structures by laminating, random fiber molding or autoclave curing. Composites were determined to be thermally stable and retain useful properties after extended exposures at 550 to 650 F. The material and fabrication capability were demonstrated by the fabrication and evaluation of prototype complex fan blades.-

Tailor making high performance graphite fiber reinforced PMR polyimides

NASA Technical Reports Server (NTRS)

Serafini, T. T.; Vannucci, R. D.

1974-01-01

Studies performed to demonstrate the feasibility of using the polymerization of monomer reactants (PMR) approach to tailor make processable polyimide matrix resins are described. Monomeric reactant solutions containing the dimethyl ester of 3,3',4,4' -benzophenonetetracarboxylic acid, 4, 4' -methylenedianiline and the monomethyl ester of 5-norbornene-2, 3-dicarboxylic acid were used to impregnate Hercules HTS graphite fiber. Six different monomeric reactant stoichiometries were studied. The processing characteristics and elevated temperature mechanical properties of the PMR polyimide/HTS graphite fiber composites are described.

Rheological properties of experimental Bis-GMA/TEGDMA flowable resin composites with various macrofiller/microfiller ratio.

PubMed

Beun, Sébastien; Bailly, Christian; Dabin, Anne; Vreven, José; Devaux, Jacques; Leloup, Gaëtane

2009-02-01

The purpose of this study was to investigate the rheological behavior of resin composites and to evaluate the influence of each component, organic as well as inorganic, on their viscoelastic properties by testing model experimental formulations. Several unfilled mixtures of 2,2-bis-[4-(methacryloxy-2-hydroxy-propoxy)-phenyl]-propane (Bis-GMA) and triethylene glycol dimethacrylate (TEGDMA) were prepared as well as experimental flowable resin composites using a Bis-GMA/TEGDMA 50/50 wt% mixture as organic fraction filled at 60% in weight with varying ratios of silanated barium glass (1 microm) and partially hydrophobic fumed silica (0.1 microm). Their rheological properties were investigated using dynamic oscillatory rheometers. Transmission electron microscopy (TEM) was also performed to investigate the spatial organization of the filler particles. Unfilled Bis-GMA/TEGDMA mixtures all showed a Newtonian behavior. The experimental flowable resin composites were non-Newtonian, shear-thinning fluids. As the quantity of microfiller increased, the viscosity increased and the shear-thinning behavior increased as well. In addition, the experimental composites showed thixotropy, i.e. their viscosity is a function of time after deformation. All these properties were not specifically linked to the creation and destruction of a visible network between inorganic particles, as no difference could be seen between particles' spatial organization at the equilibrium rest state or immediately after deformation. The complex viscoelastic properties of resin composites are due to interactions between microfiller and monomer molecules. Modifying the chemical and physical properties of the particles' surface could possibly improve their flow properties and thus their clinical handling performances.

78 FR 59653 - Notice of Scope Rulings

Federal Register 2010, 2011, 2012, 2013, 2014

2013-09-27

... Administration, U.S. Department of Commerce, 14th Street and Constitution Avenue NW., Washington, DC 20230... polytetrafluoroethylene (PTFE) resin products made from raw, unfilled PTFE powder from Russia and the People's Republic of... the antidumping duty order; April 26, 2013 (preliminary). People's Republic of China A-570-967 and C...

Advanced composites: Fabrication processes for selected resin matrix materials

NASA Technical Reports Server (NTRS)

Welhart, E. K.

1976-01-01

This design note is based on present state of the art for epoxy and polyimide matrix composite fabrication technology. Boron/epoxy and polyimide and graphite/epoxy and polyimide structural parts can be successfully fabricated. Fabrication cycles for polyimide matrix composites have been shortened to near epoxy cycle times. Nondestructive testing has proven useful in detecting defects and anomalies in composite structure elements. Fabrication methods and tooling materials are discussed along with the advantages and disadvantages of different tooling materials. Types of honeycomb core, material costs and fabrication methods are shown in table form for comparison. Fabrication limits based on tooling size, pressure capabilities and various machining operations are also discussed.

A new readily processable polyimide

NASA Technical Reports Server (NTRS)

Harris, F. W.; Beltz, M. W.; Hergenrother, P. M.

1986-01-01

As part of an effort to develop tough solvent resistance thermoplastics for potential use as structural resins on aerospace vehicles, a new processable polyimide was evaluated. The synthesis involved the reaction of a new diamine, 1,3-bis 2-(3-aminophenoxy)ethyl ether, with 3,3',4,4'-benzophenonetetracarboxylic dianhydride to form the polyamic acid and subsequent conversion of it to the polyimide. Various physical properties such as thermal stability, solvent resistance, glass transition temperature, crystalline melt temperature, melt viscosity and mechanical properties such as fracture toughness, adhesive, film and composite properties are reported. Of particular interest is the extremely high titanium to titanium tensile shear strength obtained for this polyimide.

Fiber study involving a polyimide matrix

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cano, R.J.; Rommel, M.; Hinkley, J.A.

1996-12-31

Mechanical properties are presented for eight different intermediate modulus carbon fiber/ polyimide matrix composites. Two unsized carbon fibers (Thornel T650-42 and Hercules IM9) and two sized carbon fibers (high temperature sized Thornel T650-42 HTS and epoxy sized Toray T1000) were prepregged on the NASA LaRC Multipurpose Tape Machine using the NASA LaRC developed polyimide resin matrix, LaRC{trademark}-PETI-5, and the DuPont developed Avitnid{reg_sign} R1-16. Composite panels fabricated from these prepregs were evaluated to determine their mechanical properties. The data show the effects of using sized fibers on the processing and mechanical properties of polyimide composites.

SEM/XPS analysis of fractured adhesively bonded graphite fibre surface resin-rich/graphite fibre composites

NASA Technical Reports Server (NTRS)

Devilbiss, T. A.; Wightman, J. P.; Progar, D. J.

1988-01-01

Samples of graphite fiber-reinforced polyimide were fabricated allowing the resin to accumulate at the composite surface. These surface resin-rich composites were then bonded together and tested for lap shear strength both before and after thermal aging. Lap shear strength did not appear to show a significant improvement over that previously recorded for resin-poor samples and was shown to decrease with increasing aging time and temperature.

Isothermal aging effects on PMR-15 resin

NASA Technical Reports Server (NTRS)

Bowles, Kenneth J.; Jayne, Douglas; Leonhardt, Todd A.

1992-01-01

Specimens of PMR-15 polyimide neat resin were aged in air at temperatures of 288, 316, and 343 C. Weight losses and dimensional changes were monitored during the course of the exposure time. Physical changes were also observed by optical and electron microscopy. It was found that polyimide polymer degradation occurred within a thin surface layer that developed and grew during thermal aging. The cores of the polymer specimens were protected from oxidative degradation, and they were relatively unchanged by the thermal treatment. Surface cracking was observed at 343 C and was probably due to an interaction between voids and stresses that developed in the surface layer.

Solvent Free Low-Melt Viscosity Imide Oligomers And Thermosetting Polyimide Composites

NASA Technical Reports Server (NTRS)

Chuang, CHun-Hua (Inventor)

2006-01-01

This invention relates to the composition and a solvent-free process for preparing novel imide oligomers and polymers specifically formulated with effective amounts of a dianhydride such as 2,3,3',4-biphenyltetra carboxylic dianydride (a-BPDA), at least one aromatic diamine' and an endcapped of 4-phenylethynylphthalic anhydride (PEPA) or nadic anhydride to produce imide oligomers that possess a low-melt viscosity of 1-60 poise at 260-280" C. When the imide oligomer melt is cured at about 371 C. in a press or autoclave under 100-500 psi, the melt resulted in a thermoset polyimide having a glass transition temperature (T(sub g)) equal to and above 310 C. A novel feature of this process is that the monomers; namely the dianhydrides, diamines and the endcaps, are melt processable to form imide oligomers at temperatures ranging between 232-280 C. (450-535 F) without any solvent. These low-melt imide oligomers can be easily processed by resin transfer molding (RTM), vacuum-assisted resin transfer molding (VARTM) or the resin infusion process with fiber preforms e.g. carbon, glass or quartz preforms to produce polyimide matrix composites with 288-343C (550-650 F) high temperature performance capability.

Diamines and polyimides containing pendent ethynyl groups

NASA Technical Reports Server (NTRS)

Hergenrother, Paul M. (Inventor); Jensen, Brian J. (Inventor)

1994-01-01

Diamines containing pendent ethynyl and substituted ethynyl groups are synthesized. These diamines are reacted with dianhydrides to form polyamide acids, which are chemically or thermally cyclodehydrated to form polyimides and copolyimides with pendent ethynyl groups. Upon heating, the pendent ethynyl groups react to form crosslinked resins that are useful as adhesives, composite matrices, coatings, moldings, and films.

Evaluation of Nanoclay Exfoliation Strategies for Thermoset Polyimide Nanocomposite Systems

NASA Technical Reports Server (NTRS)

Ginter, Michael J.; Jana, Sadhan C.; Miller, Sandi G.

2007-01-01

Prior works show exfoliated layered silicate reinforcement improves polymer composite properties. However, achieving full clay exfoliation in high performance thermoset polyimides remains a challenge. This study explores a new method of clay exfoliation, which includes clay intercalation by lower molecular weight PMR monomer under conditions of low and high shear and sonication, clay treatments by aliphatic and aromatic surfactants, and clay dispersion in primary, higher molecular weight PMR resin. Clay spacing, thermal, and mechanical properties were evaluated and compared with the best results available in literature for PMR polyimide systems.

Analysis of the Barrier Properties of Polyimide-Silicate Nanocomposites

NASA Technical Reports Server (NTRS)

Campbell, Sandi; Johnston, J. Chris; Inghram, Linda; McCorkle, Linda; Silverman, Edward

2003-01-01

Montmorillonite clay was organically modified and dispersed into a thermoplastic (BPADA-BAPP) and a thermosetting (PMR-15) polyimide matrix. The barrier properties of the neat resins and the nanocomposites were evaluated. Reductions in gas permeability and water absorption were observed in thermoplastic polyimide nanocomposites. The thermosetting polyimide showed a reduction in weight loss during isothermal aging at 288 C. Carbon fabric (T650-35, 8 HS, 8 ply) composites were prepared using both the BPADE-BAPP and PMR-15 based nanocomposites. Dispersion of the layered silicate in the BPADA-BAPP matrix reduced helium permeability by up to 70 percent. The PMR-15/ silicate nanocomposite matrix had an increase in thermal oxidative stability of up to 25 percent.

Kinetics of imidization and crosslinking in PMR-polyimide resin

NASA Technical Reports Server (NTRS)

Lauver, R. W.

1977-01-01

Infrared spectroscopy and differential scanning calorimetry were employed to study the imidization and crosslinking kinetics of norbornenyl-capped, addition-type polyimide resins (designated PMR for polymerization of monomer reactants). The spectral and thermal analyses were performed on resin specimens which had been isothermally aged at temperatures appropriate for imidization (120 to 204 C) and crosslinking (275 to 325 C). Imidization occurs rapidly (approximately 0.01/min) at short times, while at times longer than approximately 0.5 hour, the rate decreases significantly (approximately 0.0001/min). The crosslinking reaction exhibits first order kinetics during the initial portion of the reaction and its rate appears to be limited by the reversion of the norbornenyl Diels-Alder adduct. The total heat evolved per mole of endcap during crosslinking shows an inverse dependence on the molecular weight of the imide prepolymers. This reflects the effect of endcap dilution and decreased mobility of the larger oligomers.

Advanced thermoplastic resins, phase 2

NASA Technical Reports Server (NTRS)

Brown, A. M.; Hill, S. G.; Falcone, A.

1991-01-01

High temperature structural resins are required for use on advanced aerospace vehicles as adhesives and composite matrices. NASA-Langley developed polyimide resins were evaluated as high temperature structural adhesives for metal to metal bonding and as composite matrices. Adhesive tapes were prepared on glass scrim fabric from solutions of polyamide acids of the semicrystalline polyimide LARC-CPI, developed at the NASA-Langley Research Center. Using 6Al-4V titanium adherends, high lap shear bond strengths were obtained at ambient temperature (45.2 MPa, 6550 psi) and acceptable strengths were obtained at elevated temperature (14.0 MPa, 2030 psi) using the Pasa-Jell 107 conversion coating on the titanium and a bonding pressure of 1.38 MPa (200 psi). Average zero degree composite tensile and compressive strengths of 1290 MPa (187 ksi) and 883 MPa (128 ksi) respectively were obtained at ambient temperature with unsized AS-4 carbon fiber reinforcement.

Hybridized polymer matrix composite

NASA Technical Reports Server (NTRS)

Stern, B. A.; Visser, T.

1981-01-01

Under certain conditions of combined fire and impact, graphite fibers are released to the atmosphere by graphite fiber composites. The retention of graphite fibers in these situations is investigated. Hybrid combinations of graphite tape and cloth, glass cloth, and resin additives are studied with resin systems. Polyimide resins form the most resistant composites and resins based on simple novolac epoxies the least resistant of those tested. Great improvement in the containment of the fibers is obtained in using graphite/glass hybrids, and nearly complete prevention of individual fiber release is made possible by the use of resin additives.

Nontoxic Resins Advance Aerospace Manufacturing

NASA Technical Reports Server (NTRS)

2009-01-01

The 2008 NASA Commercial Invention of the Year, PETI-330, is a polyimide matrix resin that performs well at high temperatures and is easily processed into composites in a simple, short curing cycle. Invented by scientists at Langley Research Center, PETI-330 is now licensed to Ube Industries, based in Japan with its American headquarters in New York. In addition to being durable and lightweight, the resin is also nontoxic, which makes it safe for workers to handle. PETI-330 was created specifically for heat-resistant composites formed with resin transfer molding and resin infusion, which formerly could only be used with low temperature resin systems.

NMR Guided Design of Endcaps With Improved Oxidation Resistance

NASA Technical Reports Server (NTRS)

Meador, Mary Ann B.; Frimer, Aryeh A.

2002-01-01

A polyimide is a polymer composed of alternating units of diamine and dianhydride, linked to each other via an imide bond. PMR polyimides, commonly used in the aerospace industry, are generally capped at each end by a norbornene endcap which serves a double function: (1) It limits the number of repeating units and, hence, the average molecular weight of the various polymer chains (oligomers), thereby improving processibility; (2) Upon further treatment (curing), the endcap crosslinks the various oligomer strands into a tough heat-resistant piece. Norbornenyl-end capped PMR polyimide resins' are widely used as polymer matrix composite materials for aircraft engine applications,2 since they combine ease of processing with good oxidative stability up to 300 C. PMR resins are prepared by a twestep approach involving the initial formation of oligomeric pre-polymers capped at both ends by a latent reactive end cap. The end cap undergoes cross-linking during higher temperature processing, producing the desired low density, high specific strength materials, as shown for PMR-15.

Development of an impact- and solvent-resistant thermoplastic composite matrix, phase 4

NASA Technical Reports Server (NTRS)

Delano, C. B.

1987-01-01

Polyimides from BTDA with m-phenylenediamine and three aliphatic diamines were prepared in cresol and characterized. Characterization tests included compression strength and modulus, stressed solvent resistance, and melt-flow tests. Efforts to reduce the molecular weights of these polymers by either stoichiometric imbalance or phthalic anhydride end capping produced opacity in the polymer moldings when the stoichiometry was less than 99 percent. Use of 2,4-diaminotoluene in place of the m-phenylenediamine allowed clear polymer moldings to be obtained at all stoichiometries by end capping or stoichiometric imbalance. After melt-flow/molecular-weight studies, carbon fabric composites were prepared from three polyimide compositions containing BTDA, 2,4-diaminotoluene and two aliphatic diamines. Flexural strengths of two of the resins were in excess of 689 MPa (100 ksi) at both room temperature and 93 C. The polyimide from BTDA was selected for scale-up and neat resin characterization tests. The Tg of this polymer was 233 C.

A tough performance simultaneous semi-interpenetrating polymer network

NASA Technical Reports Server (NTRS)

Pater, Ruth H. (Inventor)

1989-01-01

A semi-interpenetrating polyimide (semi-IPN) network and methods for making and using the same are disclosed. The semi-IPN system comprises a high performance thermosetting polyimide having an acetylene-terminated group acting as a crosslinking site and a high performance linear thermoplastic polyimide. The polymer is made by combining low viscosity precursors and low molecular weight polymers of the thermosetting and thermoplastic polyimides and allowing them to react in the immediate presence of each other to form a simultaneous semi-interpenetrating polyimide network. Provided is a high temperature system having significantly improved processability and damage tolerance while maintaining excellent thermo-oxidative stability, mechanical properties and resistance to humidity, when compared with the commercial high temperature resin, Thermid 600. This material is particularly adapted for use as a molding, adhesive and advanced composite matrix for aerospace structural and electronic applications.

Influence of laser structuring of PEEK, PEEK-GF30 and PEEK-CF30 surfaces on the shear bond strength to a resin cement.

PubMed

Henriques, Bruno; Fabris, Douglas; Mesquita-Guimarães, Joana; Sousa, Anne C; Hammes, Nathalia; Souza, Júlio C M; Silva, Filipe S; Fredel, Márcio C

2018-08-01

The aim of this study was to evaluate the influence of a surface conditioning technique using laser ablation and acid etching on PEEK substrate on its bonding strength to a resin cement. Cylindrical specimens of unfilled PEEK, 30% glass fiber reinforced PEEK and 30% carbon fiber reinforced PEEK were separated in four groups according to the following surface treatments: acid etching with H 2 SO 4 , laser ablation with 200 µm holes spaced 400 µm apart (D2E4), laser ablation with 200 µm holes spaced 600 µm apart (D2E6), and laser ablation (D2E4) followed by acid etching. A dual-curing resin cement (Allcem CORE) was then applied to the PEEK surface. Specimens were aged in distilled water at 37 °C for 24 h. Shear bond strength tests were performed to the fracture of the samples. Two-way ANOVA statistical analysis was performed with a significance level of 0.05. Scanning electron microscopy analysis was performed to analyse the conditioned and fracture surfaces. SEM images of the test interfaces showed that the resin cement could not flow in the holes designed by the laser ablation on the PEEK surface. The shear bond strength of PEEK to resin cement was not improved by the surface modification of the PEEK. Also, there was a statistically significant decrease in shear bond strength for unfilled PEEK specimens. On carbon or glass reinforced PEEK, the change was not significant. SEM images of the fracture surfaces revealed that the failure mode was mainly adhesive. Although laser ablation promoted the PEEK surface modification by the formation of retentive holes, the test resin cement could not thoroughly flow on the rough modified surfaces to establish an effective mechanical interlocking. That negatively affected the shear bonding strength of PEEK to the resin cement. Further studies should be carried out to increase the bonding between PEEK and resin cements. Copyright © 2018 Elsevier Ltd. All rights reserved.

Polyimides Containing Amide And Perfluoroisopropyl Links

NASA Technical Reports Server (NTRS)

Dezem, James F.

1993-01-01

New polyimides synthesized from reactions of aromatic hexafluoroisopropyl dianhydrides with asymmetric amide diamines. Soluble to extent of at least 10 percent by weight at temperature of about 25 degrees C in common amide solvents such as N-methylpyrrolidone, N,N-dimethylacetamide, and N,N-dimethylformamide. Polyimides form tough, flexible films, coatings, and moldings. Glass-transition temperatures ranged from 300 to 365 degrees C, and crystalline melting temperatures observed between 543 and 603 degrees C. Display excellent physical, chemical, and electrical properties. Useful as adhesives, laminating resins, fibers, coatings for electrical and decorative purposes, films, wire enamels, and molding compounds.

Development of aircraft lavatory compartments with improved fire resistance characteristics. Phase 2: Sandwich panel resin system development

NASA Technical Reports Server (NTRS)

Anderson, R. A.; Arnold, D. B.; Johnson, G. A.

1979-01-01

A NASA-funded program is described which aims to develop a resin system for use in the construction of lavatory wall panels, sidewall panels, and ceiling panels possessing flammability, smoke and gas emission, and toxicity (FS&T) characteristics superior to the existing epoxy resin. Candidate resins studied were phenolic, polyimide, and bismaleimide. Based on the results of a series of FS&T as well as mechanical and aesthetic property tests, a phenolic resin was chosen as the superior material. Material and process specifications covering the phenolic resin based materials were prepared and a method of rating sandwich panel performance was developed.

Polyimide molding powder, coating, adhesive, and matrix resin

NASA Technical Reports Server (NTRS)

St.clair, Terry L. (Inventor); Progar, Donald J. (Inventor)

1992-01-01

The invention is a polyimide prepared from 3,4'-oxydianiline (3,4'-ODA) and 4,4'-oxydiphthalic anhydride (ODPA), in 2-methoxyethyl ether (diglyme). The polymer was prepared in ultra high molecular weight and in a controlled molecular weight form which has a 2.5 percent offset in stoichiometry (excess diamine) with a 5.0 percent level of phthalic anhydride as an endcap. This controlled molecular weight form allows for greatly improved processing of the polymer for moldings, adhesive bonding, and composite fabrication. The higher molecular weight version affords tougher films and coatings. The overall polymer structure groups in the dianhydride, the diamine, and a metal linkage in the diamine affords adequate flow properties for making this polymer useful as a molding powder, adhesive, and matrix resin.

An Approach to Processable Polyimides

NASA Technical Reports Server (NTRS)

Gariepy, Christopher A.; Eby, R. K.; Meador, Michael A.

1999-01-01

The use of polymer matrix composites (PMC's) in aircraft engines can lead to substantial weight savings over metals. This weight reduction correlates into better fuel economy, increased speed, and increased passenger load. Typically, high performance PMC's possess high thermal-oxidative stabilities (TOS) and high glass transition temperatures (Tg's) to withstand temperatures up to 316 C (600 F). One of the leading high temperature resins system available today is PMR-15 (Polymerization of Monomeric Reactants, MW=1500). This thermosetting polyimide utilizes addition curing through polymer endcaps which enables hand lay-up processing of carbon fiber composite parts with low void contents. However, the large amount of hand labor raises manufacturing costs and prohibits the use of PMR-15 in many aerospace applications. Resin Transfer Molding (RTM) provides an economical alternative, but it requires a melt Viscosity of less than 10(exp 3) centipoise (cP). This is much lower than the minimum melt viscosity of PMR-15 (about 10(exp 6) cP). To improve the processability of polyimides, the polymer backbone can be modified by incorporating flexible linkages, such as branching. bulky pendant groups, kinked structures, and twisted or non-coplanar moietes . The focus of this paper will be the introduction of non-coplanar biaryls into the PMR polyimide backbone to increase processability while maintaining high temperature performance.

Low toxicity high temperature PMR polyimide

NASA Technical Reports Server (NTRS)

Pater, Ruth H. (Inventor)

1992-01-01

In-situ polymerization of monomer reactants (PMR) type polyimides constitute an important class of ultra high performance composite matrix resins. PMR-15 is the best known and most widely used PMR polyimide. An object of the present invention is to provide a substantially improved high temperature PMR-15 system that exhibits better processability, toughness, and thermo-oxidative stability than PMR-15, as well as having a low toxicity. Another object is to provide new PMR polyimides that are useful as adhesives, moldings, and composite matrices. By the present invention, a new PMR polyimide comprises a mixture of the following compounds: 3,4'-oxydianiline (3,4'-ODA), NE, and BTDE which are then treated with heat. This PMR was designated LaRC-RP46 and has a broader processing window, better reproducibility of high quality composite parts, better elevated temperature mechanical properties, and higher retention of mechanical properties at an elevated temperature, particularly, at 371 C.

Resin/graphite fiber composites

NASA Technical Reports Server (NTRS)

Cavano, P. J.; Jones, R. J.; Vaughan, R. W.

1972-01-01

High temperature resin matrices suitable for use in advanced graphite fiber composites for jet engine applications were evaluated. A series of planned, sequential screening experiments with resin systems in composite form were performed to reduce the number of candidates to a single A-type polyimide resin that repetitively produced void-free, high strength and modulus composites acceptable for use in the 550 F range for 1000 hours. An optimized processing procedure was established for this system. Extensive mechanical property studies characterized this single system, at room temperature, 500 F, 550 F and 600 F, for various exposure times.

Novel Low-Melt Viscosity Polyimides for Resin Transfer Molding (RTM)

DTIC Science & Technology

2008-08-29

used no solvent in the process and the only volatile generated is water tbrmed during the imidization process. Resins were prepared as outlined below...without the use of a solvent. Due to the commercial availabilit \\ of 3,4’ -ODA, RTM370 is cheaper to manufacture than RTM 350 or RTM330. All these rcsins

High-Performance Synthetic Fibers for Composites

DTIC Science & Technology

1992-04-01

under evaluation today include polyether ether ketone , polyamide, 23 polyamideimide, polyimide, polysulfone, and polyphenylene sulfide. Epoxy resins...shrinkage under intense neutron radiation . This attribute, together with other properties of high-temperature strength, toughness, and low nuclear...and (2) liquid or solid resins cross-linked with other esters in chopped-fiber and mineral-filled molding compounds. Polyether ether ketone (PEEK) A

P-V-T Properties of Polyimides and Model Imide Compounds

NASA Technical Reports Server (NTRS)

Orwoll, Robert A.

1997-01-01

Aromatic polyimides are used as matrix resins in advanced composites, as high strength films, and as high-temperature adhesives, owing in part to their unusual thermal and chemical stability. The polyimides' desirable qualities of very high softening temperatures and negligibly small solubilities in and low permeabilities by most solvents have limited the kinds of fundamental studies that can be performed on these systems. Consequently, relationships between the molecular structure of polyimides and their bulk properties are not as well understood as might be expected given their widespread applications. In particular, the intermolecular forces in polyimides that play a critical role determining their densities, solubilities, viscosities, moduli, glass transitions, etc. are less well characterized for polyimides than for other widely used polymeric materials. The purpose of the present study is to obtain experimental data for establishing parameters that characterize the intermolecular forces in polyimides. We report here our studies on tractable low molecular-weight imides that contain the same structural features that are present in polyimide materials. We have measured equation-of-state properties and dipole moments for a variety of such systems in the liquid state. Both pure compounds and binary mixtures have been studied.

Resin/graphite fiber composites

NASA Technical Reports Server (NTRS)

Cavano, P. J.

1974-01-01

Techniques were developed that provided thermo-oxidatively stable A-type polyimide/graphite fiber composites using the approach of in situ polymerization of monomeric reactants directly on reinforcing fibers, rather than employing separately prepared prepolymer varnish. This was accomplished by simply mixing methylene dianiline and two ester-acids and applying this solution to the fibers for subsequent molding. Five different formulated molecular weight resins were examined, and an optimized die molding procedure established for the 1500 formulated molecular weight system. Extensive ultrasonic inspection of composites was successfully utilized as a technique for monitoring laminate quality. Composite mechanical property studies were conducted with this polyimide resin at room temperature and after various time exposures in a thermo-oxidative environment at 561 K (550 F), 589 K (600 F) and 617 K (650 F). It was determined that such composites have a long term life in the temperature range of 561 K to 589 K. The final phase involved the fabrication and evaluation of a series of demonstration airfoil specimens.

Dry Process for Making Polyimide/ Carbon-and-Boron-Fiber Tape

NASA Technical Reports Server (NTRS)

Belvin, Harry L.; Cano, Roberto J.; Johnston, Norman J.; Marchello, Joseph M.

2003-01-01

A dry process has been invented as an improved means of manufacturing composite prepreg tapes that consist of high-temperature thermoplastic polyimide resin matrices reinforced with carbon and boron fibers. Such tapes are used (especially in the aircraft industry) to fabricate strong, lightweight composite-material structural components. The inclusion of boron fibers results in compression strengths greater than can be achieved by use of carbon fibers alone. The present dry process is intended to enable the manufacture of prepreg tapes (1) that contain little or no solvent; (2) that have the desired dimensions, fiber areal weight, and resin content; and (3) in which all of the fibers are adequately wetted by resin and the boron fibers are fully encapsulated and evenly dispersed. Prepreg tapes must have these properties to be useable in the manufacture of high-quality composites by automated tape placement. The elimination of solvent and the use of automated tape placement would reduce the overall costs of manufacturing.

Heat, Moisture and Chemical Resistant Polyimide Compositions and Methods for Making and Using Them

NASA Technical Reports Server (NTRS)

Pater, Ruth H. (Inventor)

2004-01-01

Polyimides having a desired combination of high thermo-oxidative stability, low moisture absorption and excellent chemical and corrosion resistance are prepared by reacting a mixture of compounds including (a) 3,3',4,4'- benzophenonetetracarboxylic dianhydride (BTDA), (b) 3,4'- oxydianiline (3,4'-ODA), and (c) 5-norbornene-2,3- dicarboxylic anhydride (NA) in a high boiling, aprotic solvent to give 5 to 35% by weight of polyamic acid solution. The ratio of (a), (b), and (c) is selected to afford a family of polyimides having different molecular weights and properties. The mixture first forms a polyamic acid precursor. Upon heating at or above 300 C, the polyamic acids form polyimides, which are particularly suitable for use as a high temperature coating, adhesive, thin film, or composite matrix resin.

Tensile bond strength of filled and unfilled adhesives to dentin.

PubMed

Braga, R R; Cesar, P F; Gonzaga, C C

2000-04-01

To determine the tensile bond strength of three filled and two unfilled adhesives applied to bovine dentin. Fragments of the labial dentin of bovine incisors were embedded in PVC cylinders with self-cure acrylic resin, and ground flat using 200 grit and 600 grit sandpaper. The following adhesive systems were tested (n=10): Prime & Bond NT, Prime & Bond NT dual cure, Prime & Bond 2.1, OptiBond Solo and Single Bond. A 3 mm-diameter bonding surface was delimited using a perforated adhesive tape. After etching with 37% phosphoric acid and adhesive application, a resin-based composite truncated cone (TPH, shade A3) was built. Tensile test was performed after 24 hrs storage in distilled water at 37 degrees C. Failure mode was accessed using a x10 magnification stereomicroscope. Weibull statistical analysis revealed significant differences in the characteristic strength between Single Bond and Prime & Bond NT dual cure, and between Single Bond and Prime & Bond 2.1. The Weibull parameter (m) was statistically similar among the five groups. Single Bond and Prime & Bond NT showed areas of dentin cohesive failure in most of the specimens. For OptiBond Solo, Prime & Bond NT dual cure and Prime & Bond 2.1 failure was predominantly adhesive.

Preparation, testing, and delivery of low density polyimide foam panels

NASA Technical Reports Server (NTRS)

Ball, G. L., III; Post, L. K.; Salyer, I. O.

1975-01-01

Plastic foams based on polyimide resins were shown to be stable at relatively high temperatures, and to possess very low flame spread and smoke generation characteristics. A system and process were developed to prepare low-density polyimide foam from a liquid formulation. The system is based on the reaction of micropulverized grade pyromellitic dianhydride with a polymeric diisocyanate. The panels produced were postcured at elevated temperatures to achieve maximum thermal and fire resistance, and incorporation of a fire retardant into the formulation was considered. The effects of a flame retardant (Flameout 5600B1) were investigated, but eliminated in preference to the postcuring approach.

Tackifier for addition polyimides containing monoethylphthalate

NASA Technical Reports Server (NTRS)

St.clair, T. L.; Butler, J. M. (Inventor)

1981-01-01

An improvement of addition polyimides wherein an essentially solventless, high viscosity laminating resin is synthesized from low cost liquid monomers is disclosed. The improved process takes advantage of a reactive, liquid plasticizer such as monoethylphthalate (MEP) which is used in lieu of an alcohol solvent, and helps solve a major problem of maintaining good prepreg tack and drape, or the ability of the prepreg to adhere to adjacent plies and conform to a desired shape during the layup process. This improvement results in both longer life of the polymer prepreg and the processing of low void laminate and appears to be applicable to all addition polyimide systems.

Polyimides Containing Pendent Phosphine Oxide Groups for Space Applications

NASA Technical Reports Server (NTRS)

Thompson, C. M.; Smith, J. G., Jr.; Watson, K. A.; Connell, J. W.

2002-01-01

As part of an ongoing materials development activity to produce high performance polymers that are durable to the space environment, phosphine oxide containing polyimides have been under investigation. A novel dianhydride was prepared from 2,5-dihydroxyphenyldiphenylphosphine oxide in good yield. The dianhydride was reacted with commercially available diamines, and a previously reported diamine was reacted with commercially available dianhydrides to prepare isomeric polyimides. The physical and mechanical properties, particularly thermal and optical properties, of the polymers were determined. One material exhibited a high glass transition temperature, high tensile properties, and low solar absorptivity. The chemistry, physical, and mechanical properties of these resins will be discussed.

Characterization of PMR polyimide resin and prepreg

NASA Technical Reports Server (NTRS)

Lindenmeyer, P. H.; Sheppard, C. H.

1984-01-01

Procedures for the chemical characterization of PMR-15 resin solutions and graphite-reinforced prepregs were developed, and a chemical data base was established. In addition, a basic understanding of PMR-15 resin chemistry was gained; this was translated into effective processing procedures for the production of high quality graphite composites. During the program the PMR monomers and selected model compounds representative of postulated PMR-15 solution chemistry were acquired and characterized. Based on these data, a baseline PMR-15 resin was formulated and evaluated for processing characteristics and composite properties. Commercially available PMR-15 resins were then obtained and chemically characterized. Composite panels were fabricated and evaluated.

Fabrication of Superconducting Quantum Interference Device Magnetometers on a Glass Epoxy Polyimide Resin Substrate with Copper Terminals

NASA Astrophysics Data System (ADS)

Kawai, Jun; Kawabata, Miki; Oyama, Daisuke; Uehara, Gen

We have developed fabrication technique of superconducting quantum interference device (SQUID) magnetometers based on Nb/AlAlOx/Nb junctions directly on a glass epoxy polyimide resin substrate, which has copper terminals embedded in advance. The advantage of this method is that no additional substrate and wirebonds are needed for assembly. Compared to conventional SQUID magnetometers, which are assembled with a SQUID chip fabricated on a Si substrate and wirebonding technique, low risk of disconnection can be expected. A directly-coupled multi-loop SQUID magnetometer fabricated with this method has as good noise performance as a SQUID magnetometer with the same design fabricated on a Si wafer. The magnetometer sustained its performance through thermal cycle test 13 times so far.

Catalytic trimerization of aromatic nitriles for synthesis of polyimide matrix resins

NASA Technical Reports Server (NTRS)

Hsu, L. C.

1974-01-01

Aromatic nitriles may be trimerized at moderate temperature and pressure with p-toluenesulfonic acid as catalyst. Studies were conducted to establish the effect of the reaction temperature, pressure, time, and catalyst concentration on yield of the trimerized product. Trimerization studies were also conducted to establish the effect of substituting electron donating or withdrawing groups on benzonitrile. Preliminary results of using the catalytic trimerization approach to prepare s-triazine cross-linked polyimide/graphite fiber composites are presented.

Development of fire-resistant, low smoke generating, thermally stable end items for commercial aircraft and spacecraft using a basic polyimide resin

NASA Technical Reports Server (NTRS)

Gagliani, J.; Lee, R.; Sorathia, U. A.; Wilcoxson, A. L.

1980-01-01

A terpolyimide precursor was developed which can be foamed by microwave methods and yields foams possessing the best seating properties. A continuous process, based on spray drying techniques, permits production of polyimide powder precursors in large quantities. The constrained rise foaming process permits fabrication of rigid foam panels with improved mechanical properties and almost unlimited density characteristics. Polyimide foam core rigid panels were produced by this technique with woven fiberglass fabric bonded to each side of the panel in a one step microwave process. The fire resistance of polyimide foams was significantly improved by the addition of ceramic fibers to the powder precursors. Foams produced from these compositions are flexible, possess good acoustical attenuation and meet the minimum burnthrough requirements when impinged by high flux flame sources.

High temperature resin matrix composites for aerospace structures

NASA Technical Reports Server (NTRS)

Davis, J. G., Jr.

1980-01-01

Accomplishments and the outlook for graphite-polyimide composite structures are briefly outlined. Laminates, skin-stiffened and honeycomb sandwich panels, chopped fiber moldings, and structural components were fabricated with Celion/LARC-160 and Celion/PMR-15 composite materials. Interlaminar shear and flexure strength data obtained on as-fabricated specimens and specimens that were exposed for 125 hours at 589 K indicate that epoxy sized and polyimide sized Celion graphite fibers exhibit essentially the same behavior in a PMR-15 matrix composite. Analyses and tests of graphite-polyimide compression and shear panels indicate that utilization in moderately loaded applications offers the potential for achieving a 30 to 50 percent reduction in structural mass compared to conventional aluminum panels. Data on effects of moisture, temperature, thermal cycling, and shuttle fluids on mechanical properties indicate that both LARC-160 and PMR-15 are suitable matrix materials for a graphite-polyimide aft body flap. No technical road blocks to building a graphite-polyimide composite aft body flap are identified.

Testing of molded high temperature plastic actuator road seals for use in advanced aircraft hydraulic systems

NASA Technical Reports Server (NTRS)

Waterman, A. W.; Huxford, R. L.; Nelson, W. G.

1976-01-01

Molded high temperature plastic first and second stage rod seal elements were evaluated in seal assemblies to determine performance characteristics. These characteristics were compared with the performance of machined seal elements. The 6.35 cm second stage Chevron seal assembly was tested using molded Chevrons fabricated from five molding materials. Impulse screening tests conducted over a range of 311 K to 478 K revealed thermal setting deficiencies in the aromatic polyimide molding materials. Seal elements fabricated from aromatic copolyester materials structurally failed during impulse cycle calibration. Endurance testing of 3.85 million cycles at 450 K using MIL-H-83283 fluid showed poorer seal performance with the unfilled aromatic polyimide material than had been attained with seals machined from Vespel SP-21 material. The 6.35 cm first stage step-cut compression loaded seal ring fabricated from copolyester injection molding material failed structurally during impulse cycle calibration. Molding of complex shape rod seals was shown to be a potentially controllable technique, but additional molding material property testing is recommended.

Graphite/Polyimide Composites Subjected to Biaxial Loads at Elevated Temperatures

NASA Technical Reports Server (NTRS)

Kumosa, Maciej S.; Sutter, J. K.

2007-01-01

First, we will review our most important research accomplishments from a five year study concerned with the prediction of mechanical properties of unidirectional and woven graphite/polyimide composites based on T650-35, M40J and M60J fibers embedded in either PMR-15 or PMR-II-50 polyimide resins. Then, an aging model recently developed for the composites aged in nitrogen will be proposed and experimentally verified on an eight harness satin (8HS) woven T650-35/PMR-15 composite aged in nitrogen at 315 C for up to 1500 hours. The study was supported jointly between 1999 and 2005 by the AFOSR, the NASA Glenn Research Center, and the National Science Foundation.

Tackifier for addition polyimides

NASA Technical Reports Server (NTRS)

Butler, J. M.; St.clair, T. L.

1980-01-01

A modification to the addition polyimide, LaRC-160, was prepared to improve tack and drape and increase prepeg out-time. The essentially solventless, high viscosity laminating resin is synthesized from low cost liquid monomers. The modified version takes advantage of a reactive, liquid plasticizer which is used in place of solvent and helps solve a major problem of maintaining good prepeg tack and drape, or the ability of the prepeg to adhere to adjacent plies and conform to a desired shape during the lay up process. This alternate solventless approach allows both longer life of the polymer prepeg and the processing of low void laminates. This approach appears to be applicable to all addition polyimide systems.

Polyimide resin composites via in situ polymerization of monomeric reactants

NASA Technical Reports Server (NTRS)

Cavano, P. J.

1974-01-01

Thermo-oxidatively stable polyimide/graphite-fiber composites were prepared using a unique in situ polymerization of monomeric reactants directly on reinforcing fibers. This was accomplished by using an aromatic diamine and two ester-acids in a methyl alcohol solvent, rather than a previously synthesized prepolymer varnish, as with other A-type polyimides. A die molding procedure was developed and a composite property characterization conducted with high modulus graphite fiber tow. Flexure, tensile, compressive, and shear tests were conducted at temperatures from 72 to 650 F on laminates before and after exposures at the given temperatures in an air environment for times up to 1000 hours. The composite material was determined to be oxidatively, thermally, and hydrolytically stable.

Low Melt Viscosity Resins for Resin Transfer Molding

NASA Technical Reports Server (NTRS)

Harris, Frank W.

2002-01-01

In recent years, resin transfer molding (RTM) has become one of the methods of choice for high performance composites. Its cost effectiveness and ease of fabrication are major advantages of RTM. RTM process usually requires resins with very low melt viscosity (less than 10 Poise). The optimum RTM resins also need to display high thennal-oxidative stability, high glass transition temperature (T(sub g)), and good toughness. The traditional PMR-type polyimides (e.g. PMR-15) do not fit this requirement, because the viscosities are too high and the nadic endcap cures too fast. High T(sub g), low-melt viscosity resins are highly desirable for aerospace applications and NASA s Reusable Launch Vehicle (RLV) program. The objective of this work is to prepare low-melt viscosity polyimide resins for RTM or resin film infusion (RFI) processes. The approach involves the synthesis of phenylethynyl-terminated imide oligomers. These materials have been designed to minimize their melt viscosity so that they can be readily processed. During the cure, the oligomers undergo both chain extension and crosslinking via the thermal polymerization of the phenylethynyl groups. The Phenylethynyl endcap is preferred over the nadic group due to its high curing temperature, which provides broader processing windows. This work involved the synthesis and polymerization of oligomers containing zig-zag backbones and twisted biphenyl structures. Some A-B type precursors which possessed both nitro and anhydride functionality, or both nitro and amine functionality, were also synthesized in order to obtain the well defined oligomers. The resulting zig-zag structured oligomers were then end-capped with 4-phenylethynylphthalic anhydride (PEPA) for further cure. The properties of these novel imide oligomers are evaluated.

Development of lightweight reinforced plastic laminates for spacecraft interior applications

NASA Technical Reports Server (NTRS)

Hertz, J.

1975-01-01

Lightweight, Kevlar - reinforced laminating systems that are non-burning, generate little smoke in the space shuttle environment, and are physically equivalent to the fiberglass/polyimide system used in the Apollo program for non-structural cabin panels, racks, etc. Resin systems representing five generic classes were screened as matrices for Kevlar 49 reinforced laminates. Of the systems evaluated, the polyimides were the most promising with the phenolics a close second. Skybond 703 was selected as the most promising resin candidate. With the exception of compression strength, all program goals of physical and mechanical properties were exceeded. Several prototype space shuttle mobility and translation handrail segments were manufactured using Kevlar/epoxy and Kevlar-graphite/epoxy. This application shows significant weight savings over the baseline aluminum configuration used previous. The hybrid Kevlar-graphite/epoxy is more suitable from a processing standpoint.

New addition curing polyimides

NASA Technical Reports Server (NTRS)

Frimer, Aryeh A.; Cavano, Paul

1991-01-01

In an attempt to improve the thermal-oxidative stability (TOS) of PMR-type polymers, the use of 1,4-phenylenebis (phenylmaleic anhydride) PPMA, was evaluated. Two series of nadic end-capped addition curing polyimides were prepared by imidizing PPMA with either 4,4'-methylene dianiline or p-phenylenediamine. The first resulted in improved solubility and increased resin flow while the latter yielded a compression molded neat resin sample with a T(sub g) of 408 C, close to 70 C higher than PME-15. The performance of these materials in long term weight loss studies was below that of PMR-15, independent of post-cure conditions. These results can be rationalized in terms of the thermal lability of the pendant phenyl groups and the incomplete imidization of the sterically congested PPMA. The preparation of model compounds as well as future research directions are discussed.

Low pressure process for continuous fiber reinforced polyamic acid resin matrix composite laminates

NASA Technical Reports Server (NTRS)

Druyun, Darleen A. (Inventor); Hou, Tan-Hung (Inventor); Kidder, Paul W. (Inventor); Reddy, Rakasi M. (Inventor); Baucom, Robert M. (Inventor)

1994-01-01

A low pressure processor was developed for preparing a well-consolidated polyimide composite laminate. Prepreg plies were formed from unidirectional fibers and a polyamic acid resin solution. Molding stops were placed at the sides of a matched metal die mold. The prepreg plies were cut shorter than the length of the mold in the in-plane lateral direction and were stacked between the molding stops to a height which was higher than the molding stops. The plies were then compressed to the height of the stops and heated to allow the volatiles to escape and to start the imidization reaction. After removing the stops from the mold, the heat was increased and 0 - 500 psi was applied to complete the imidization reaction. The heat and pressure were further increased to form a consolidated polyimide composite laminate.

Reflective Silvered Polyimide Films Via In Situ Thermal Reduction Silver (I) Complexes

NASA Technical Reports Server (NTRS)

Southward, Robin E. (Inventor); Thompson, David W. (Inventor); St.Clair, Anne K. (Inventor); Stoakley, Diane M. (Inventor)

2000-01-01

Self-metallizing. flexible polyimide films with highly reflective surfaces are prepared by an in situ self-metallization procedure involving thermally initiated reduction of polymer-soluble silver(I) complexes. Polyamic acid solutions are doped with silver(I) acetate and solubilizing agents. Thermally curing the silver(I) doped resins leads to flexible. metallized films which have reflectivities as high as 100%. abrasion-resistant surfaces. thermal stability and, in some cases, electrical conductivity, rendering them useful for space applications.

Effect of matrix material on the fracture behavior and toughness of high temperature polymer composites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chenock, T.A.Jr.; Heshmet, A.

1990-07-01

The effect of matrix material on the strength, toughness, and fracture behavior of two high temperature polyimide/carbon fiber composites has been studied and compared. The polyimide matrix resins under investigation are PMR-II-20, PMR-15. Each system was reinforced with epoxy sized Celion G30-500 carbon fabric (8HSW, 3K tow). Un-notched and notched specimens were tested under 4-point bend loading in both translaminar and crosslaminar directions.

PMR polyimide/graphite fiber composite fan blades

NASA Technical Reports Server (NTRS)

Cavano, P. J.; Winters, W. E.

1976-01-01

Ultrahigh speed fan blades, designed in accordance with the requirements of an ultrahigh tip speed blade axial flow compressor, were fabricated from a high strength graphite fiber tow and a PMR polyimide resin. The PMR matrix was prepared by combining three monomeric reactants in methyl alcohol, and the solution was applied directly to the reinforcing fiber for subsequent in situ polymerization. Some of the molded blades were completely finished by secondary bonding of root pressure pads and an electroformed nickel leading edge sheath prior to final machining. The results of the spin testing of nine PMR fan blades are given. Prior to blade fabrication, heat resin tensile properties of the PMR resin were examined at four formulated molecular weight levels. Additionally, three formulated molecular weight levels were investigated in composite form with both a high modulus and a high strength fiber, both as-molded and postcured, in room temperature and 232 C transverse tensile, flexure and short beam shear. Mixed fiber orientation panels simulating potential blade constructions were also evaluated. Flexure tests, short beam shear tests, and tensile tests were conducted on these angle-plied laminates.

Evaluation of RTM370 Polyimide Composites by Resin Film Infusion (RFI)

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.; Yip, Thomas A.; Kollmansberger, Ronald B.; Tsotsis, Thomas K.

2014-01-01

RTM370 imide oligomer based on 2,3,3',4'-biphenyl dianhydride (a-BPDA), 3,4'-oxydianiline (3,4'-ODA) and terminated with the 4-phenylethynylphthalic (PEPA) endcap has been shown to exhibit a low melt viscosity (10-30 poise) at 280 C with a pot-life of 1-2 h and a high cured glass-transition temperature (Tg) of 370 C. RTM370 resin has been successfully infused into fiberglass-stitched T650-35 carbon-fabric preforms (ranged from 3- to 6-mm thick) by resin film infusion (RFI). The resulting composite panels were inspected by ultrasonic C-scan and by photomicrographs before and after post-curing as a quality control. Mechanical tests such as unnotched compression (UNC), open-hole compression (OHC), and short-beam shear strength (SBS) at ambient and elevated temperatures were performed before and after isothermal aging at 288 C for 1000 h to assess high-temperature performance. Thermal cycling of RTM370 stitched composites was also conducted from -54 C to 288 C for up to 1600 cycles to evaluate the microcrack resistance of RTM370 polyimide composites fabricated by RFI.

Modified Epoxy Adhesives and Primers

DTIC Science & Technology

1992-06-30

Shear Stress max Bulk Resin (MPa) Control 66.52±3.1 100 67.84 ±23 +20 VCDHAA 79.59 ±2.8 120 78.18 ±2.6 +15 CTBN 51.81 ±3.8 78 53.88 ±2.4 +15 CTBN ...unlimited. 0 3. ABSTRACT (MaX,UM, wor At range of monepoxy additives for epoxy resins , and non-reactive additives for3 polyimides, have been examined...a modified failure mechanism. These properties of the bulk resin translate into modest improvements in adhesive bond performance, particularly for low

High-Performance, Semi-Interpenetrating Polymer Network

NASA Technical Reports Server (NTRS)

Pater, Ruth H.; Lowther, Sharon E.; Smith, Janice Y.; Cannon, Michelle S.; Whitehead, Fred M.; Ely, Robert M.

1992-01-01

High-performance polymer made by new synthesis in which one or more easy-to-process, but brittle, thermosetting polyimides combined with one or more tough, but difficult-to-process, linear thermoplastics to yield semi-interpenetrating polymer network (semi-IPN) having combination of easy processability and high tolerance to damage. Two commercially available resins combined to form tough, semi-IPN called "LaRC-RP49." Displays improvements in toughness and resistance to microcracking. LaRC-RP49 has potential as high-temperature matrix resin, adhesive, and molding resin. Useful in aerospace, automotive, and electronic industries.

Long term isothermal aging and thermal analysis of N-CYCAP polyimides

NASA Technical Reports Server (NTRS)

Sutter, James K.; Waters, John F.; Schverman, Marla A.

1991-01-01

The N-CYCAP polyimides utilize a (2,2) paracyclophane endcap that polymerizes and does not generate volatile gases during the cure process. These polyimides have both high glass temperatures (390 C) and an onset of decomposition in air of 560 C. Thermal oxidative stability (TOS) weight loss studies show that replacing 25 percent by weight of the paraphenylene diamine in the polymer backbone with metaphenylene diamine improves the weight loss characteristics. N-CYCAP neat resin samples performed better than PMR-II-50 when exposed at 343 and 371 C in air for up to 1000 hours. Preliminary composite studies show that both PMR-II-50 and N-CYCAP have better thermal stability when fabricated on T-40R. Higher isothermal aging temperatures of longer aging times are needed to determine the differences in TOS between composite samples of PMR-II-50 and N-CYCAP polyimides.

Alternative High Performance Polymers for Ablative Thermal Protection Systems

NASA Technical Reports Server (NTRS)

Boghozian, Tane; Stackpoole, Mairead; Gonzales, Greg

2015-01-01

Ablative thermal protection systems are commonly used as protection from the intense heat during re-entry of a space vehicle and have been used successfully on many missions including Stardust and Mars Science Laboratory both of which used PICA - a phenolic based ablator. Historically, phenolic resin has served as the ablative polymer for many TPS systems. However, it has limitations in both processing and properties such as char yield, glass transition temperature and char stability. Therefore alternative high performance polymers are being considered including cyanate ester resin, polyimide, and polybenzoxazine. Thermal and mechanical properties of these resin systems were characterized and compared with phenolic resin.

Composite Materials

NASA Technical Reports Server (NTRS)

1988-01-01

Langley Research Center researchers invented an advanced polymer, a chemical compound formed by uniting many small molecules to create a complex molecule with different chemical properties. The material is a thermoplastic polyimide that resists solvents. Other polymers of this generic type are soluble in solvents, thus cannot be used where solvents are present. High Technology Services (HTS), Inc. licensed technology and is engaged in development and manufacture of high performance plastics, resins and composite materials. Techimer Materials Division is using technology for composite matrix resins that offer heat resistance and protection from radiation, electrical and chemical degradation. Applications of new polymer include molding resins, adhesives and matrix resins for fiber reinforced composites.

Processing and Properties of Vacuum Assisted Resin Transfer Molded Phenylethynyl Terminated Imide Composites

NASA Technical Reports Server (NTRS)

Cano, Roberto J.; Ghose, Sayata; Watson, Kent A.; Chunchu, Prasad B.; Jensen, Brian J.; Connell, John W.

2012-01-01

Polyimide composites are very attractive for applications that require a high strength to weight ratio and thermal stability. Recent work at NASA Langley Research Center (LaRC) has concentrated on developing new polyimide resin systems that can be processed without the use of an autoclave for advanced aerospace applications. Due to their low melt viscosities and long melt stability, certain phenylethynyl terminated imides (PETI) can be processed into composites using high temperature vacuum assisted resin transfer molding (HT-VARTM). VARTM has shown the potential to reduce the manufacturing cost of composite structures. In the current study, two PETI resins, LARC(Trademark) PETI-330 and LARC(Trademark) PETI-9, were infused into carbon fiber preforms at 260 C and cured at temperatures up to 371 C. Photomicrographs of polished cross sections were taken and void contents, determined by acid digestion, were below 4.5%. Mechanical properties including short block compression (SBC), compression after impact (CAI), and open hole compression (OHC) were determined at room temperature, 177 C, and 288 C. Both PETI-9 and PETI-330 composites demonstrated very good retention of mechanical properties at elevated temperatures. SBC and OHC properties after aging for 1000 hours at temperatures up to 288 C were also determined.

Viscoelastic properties of addition-cured polyimides used in high temperature polymer matrix composites

NASA Technical Reports Server (NTRS)

Roberts, Gary D; Malarik, Diane C.; Robaidek, Jerrold O.

1991-01-01

Viscoelastic properties of the addition cured polyimide, PMR-15, were studied using dynamic mechanical and stress relaxation tests. For temperatures below the glass transition temperature, T sub g, the dynamic mechanical properties measured using a temperature scan rate of 10 C/min were strongly affected by the presence of absorbed moisture in the resin. Dynamic mechanical properties measured as a function of time during an isothermal hold provided an indication of chemical changes occurring in the resin. For temperatures above (T sub g + 20 C), the storage modulus increased continuously as a function of time indicating that additional crosslinking is occurring in the resin. Because of these changes in chemical structures, the stress relaxation modulus could not be measured over any useful time interval for temperatures above T sub g. For temperatures below T sub g, dynamic mechanical properties appeared to be unaffected by chemical changes for times exceeding 1 hr. Since the duration of the stress relaxation tests was less than 1 hr, the stress relaxation modulus could be measured. As long as the moisture content of the resin was less than 2 pct, stress relaxation curves measured at different temperatures could be superimposed using horizontal shifts along the log(time) axis with only small shifts along the vertical axis.

Development of an impact- and solvent-resistant thermoplastic composite matrix, phase 3

NASA Technical Reports Server (NTRS)

Delano, C. B.; Kiskiras, C. J.

1985-01-01

The polyimide from BTDA 1,6-hexanediamine and m-phenylenediamine was selected from a prior study for the present study. Methods to prepare prepreg which would provide low void composites at low molding pressures from the thermoplastic polyimide were studied. Cresol solutions of the polyimide were applied to a balanced weave carbon fabric and the cresol removed prior to composite molding. Low void composites were prepared from smoothed prepregs at high pressures (34.5 MPa) and temperatures as low as 260 C. Lower molding pressures lead to higher void composites. Need for a lower melt viscosity in the neat resin is suggested as a requirement to achieve low void composites at low pressures. Some mechanical properties are included.

Rigid closed-cell polyimide foams for aircraft applications and foam-in-place technology

NASA Technical Reports Server (NTRS)

Gagliani, J.; Straub, P.; Gagliani, J., Jr.

1983-01-01

Significant accomplishments generated are summarized. Testing of closed cell foams, which has resulted in the characterization of compositions which produce rigid foams for use in galley structure applications is reported. It is shown that the density, compressive strength and shear strength of the foams are directly related to the concentrations of the microballoons. The same properties are also directly related to the resin loading. Prototype samples of rigid closed cell foams meeting the requirements of the program were submitted. Investigation of the apparatus to produce polyimide foams using foam in place techniques, resulted in the selection of a spray gun apparatus, capable to deliver a mixture of microballoons and resin binder on substrates which cures to yield a closed cell foam. It is found that the adhesion of the foam on aluminum, titanium and steel substrates is satisfactory. It is concluded that the material meets the mechanical and thermal requirements of the program.

Analyses of moisture in polymers and composites

NASA Technical Reports Server (NTRS)

Ryan, L. E.; Vaughan, R. W.

1980-01-01

A suitable method for the direct measurement of moisture concentrations after humidity/thermal exposure on state of the art epoxy and polyimide resins and their graphite and glass fiber reinforcements was investigated. Methods for the determination of moisture concentration profiles, moisture diffusion modeling and moisture induced chemical changes were examined. Carefully fabricated, precharacterized epoxy and polyimide neat resins and their AS graphite and S glass reinforced composites were exposed to humid conditions using heavy water (D20), at ambient and elevated temperatures. These specimens were fixtured to theoretically limit the D20 permeation to a unidirectional penetration axis. The analytical techniques evaluated were: (1) laser pyrolysis gas chromatography mass spectrometry; (2) solids probe mass spectrometry; (3) laser pyrolysis conventional infrared spectroscopy; and (4) infrared imaging thermovision. The most reproducible and sensitive technique was solids probe mass spectrometry. The fabricated exposed specimens were analyzed for D20 profiling after humidity/thermal conditioning at three exposure time durations.

Polyimide Composites Based on Asymmetric Dianhydrides (a-ODPA vs a-BPDA)

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.; Criss, James M.; Mintz, Eric A.

2009-01-01

RTM Resins based on a-ODPA and a-BPDA with kinked diamines exhibit low-melt viscosity (approximately 10 poise). Composites made from a-ODPA resins (T(sub g) = 265-330 C) by RTM display good mechanical properties at 288 C (550 F), but soften at 315 C (600 F). Composites of RTM370 based on a-BPDA retain excellent mechanical properties at 315 C, exceeding BMI-5270-1 capability.

Development and demonstration of manufacturing processes for fabricating graphite/Larc-160 polyimide structural elements, part 4, paragraph B

NASA Technical Reports Server (NTRS)

1981-01-01

Progress in the development of processes for production of Celion/LARC-160 graphite-polyimide materials, quality control, and the fabrication of Space Shuttle composite structure components is reported. Liquid chromatographic analyses of three repeatibility batches were performed and are compared to previous Hexcel standard production and to variables study LARC-160 intermediate resins. Development of processes for chopped fiber molding are described and flexural strength, elastic modulus, and other physical and mechanical properties of the molding are presented.

Quantitative analysis of PMR-15 polyimide resin by HPLC

NASA Technical Reports Server (NTRS)

Roberts, Gary D.; Lauver, Richard W.

1987-01-01

The concentration of individual components and of total solids of 50 wt pct PMR-15 resin solutions was determined using reverse-phase HPLC to within + or - 8 percent accuracy. Acid impurities, the major source of impurities in 3,3', 4,4'-benzophenonetetracarboxylic acid (BTDE), were eliminated by recrystallizing the BTDE prior to esterification. Triester formation was not a problem because of the high rate of esterification of the anhydride relative to that of the carboxylic acid. Aging of PMR-15 resin solutions resulted in gradual formation of the mononadimide and bisnadimide of 4,4'-methylenedianiline, with the BTDE concentration remaining constant. Similar chemical reactions occurred at a reduced rate in dried films of PMR-15 resin.

Textile composite fuselage structures development

NASA Technical Reports Server (NTRS)

Jackson, Anthony C.; Barrie, Ronald E.; Chu, Robert L.

1993-01-01

Phase 2 of the NASA ACT Contract (NAS1-18888), Advanced Composite Structural Concepts and Materials Technology for Transport Aircraft Structures, focuses on textile technology, with resin transfer molding or powder coated tows. The use of textiles has the potential for improving damage tolerance, reducing cost and saving weight. This program investigates resin transfer molding (RTM), as a maturing technology for high fiber volume primary structures and powder coated tows as an emerging technology with a high potential for significant cost savings and superior structural properties. Powder coated tow technology has promise for significantly improving the processibility of high temperature resins such as polyimides.

Polyimide Resins Resist Extreme Temperatures

NASA Technical Reports Server (NTRS)

2009-01-01

Spacecraft and aerospace engines share a common threat: high temperature. The temperatures experienced during atmospheric reentry can reach over 2,000 F, and the temperatures in rocket engines can reach well over 5,000 F. To combat the high temperatures in aerospace applications, Dr. Ruth Pater of Langley Research Center developed RP-46, a polyimide resin capable of withstanding the most brutal temperatures. The composite material can push the service temperature to the limits of organic materials. Designed as an environmentally friendly alternative to other high-temperature resins, the RP-46 polyimide resin system was awarded a 1992 "R&D 100" award, named a "2001 NASA Technology of the Year," and later, due to its success as a spinoff technology, "2004 NASA Commercial Invention of the Year." The technology s commercial success also led to its winning the Langley s "Paul F. Holloway Technology Transfer Award" as well as "Richard T. Whitcom Aerospace Technology Transfer Award" both for 2004. RP-46 is relatively inexpensive and it can be readily processed for use as an adhesive, composite, resin molding, coating, foam, or film. Its composite materials can be used in temperatures ranging from minus 150 F to 2,300 F. No other organic materials are known to be capable of such wide range and extreme high-temperature applications. In addition to answering the call for environmentally conscious high-temperature materials, RP-46 provides a slew of additional advantages: It is extremely lightweight (less than half the weight of aluminum), chemical and moisture resistant, strong, and flexible. Pater also developed a similar technology, RP-50, using many of the same methods she used with RP-46, and very similar in composition to RP-46 in terms of its thermal capacity and chemical construction, but it has different applications, as this material is a coating as opposed to a buildable composite. A NASA license for use of this material outside of the Space Agency as well as additional government-funded testing proved that RP-46 is even more exceptional than originally thought.

Interlaminar shear properties of graphite fiber, high-performance resin composites

NASA Technical Reports Server (NTRS)

Needles, H. L.; Kourtides, D. A.; Fish, R. H.; Varma, D. S.

1983-01-01

Short beam testing was used to determine the shear properties of laminates consisting of T-300 and Celion 3000 and 6000 graphite fibers, in epoxy, hot melt and solvent bismaleimide, polyimide and polystyrylpyridine (PSP). Epoxy, composites showed the highest interlaminar shear strength, with values for all other resins being substantially lower. The dependence of interlaminar shear properties on the fiber-resin interfacial bond and on resin wetting characteristics and mechanical properties is investigated, and it is determined that the lower shear strength of the tested composites, by comparison with epoxy resin matrix composites, is due to their correspondingly lower interfacial bond strengths. An investigation of the effect of the wettability of carbon fiber tow on shear strength shows wetting variations among resins that are too small to account for the large shear strength property differences observed.

The impact of hydrofluoric acid etching followed by unfilled resin on the biaxial strength of a glass-ceramic.

PubMed

Posritong, Sumana; Borges, Alexandre Luiz Souto; Chu, Tien-Min Gabriel; Eckert, George J; Bottino, Marco A; Bottino, Marco C

2013-11-01

To evaluate the null hypotheses that hydrofluoric (HF) acid etching time would neither decrease the biaxial flexural strength of a glass-based veneering ceramic nor enhance it after silane and unfilled resin (UR) applications. Disc-shaped IPS e.max ZirPress specimens were allocated into 12 groups: G1-control (no-etching), G2-30 s, G3-60 s, G4-90 s, G5-120 s, G6-60 s+60 s. Groups (G7-G12) were treated in the same fashion as G1-G6, but followed by silane and UR applications. Surface morphology and roughness (Ra and Rq) of the ceramics were assessed by means of scanning electron microscopy (SEM) and profilometry, respectively. Flexural strength was determined by biaxial testing. Data were analyzed by two-way ANOVA and the Sidak test (α=0.05). Weibull statistics were estimated and finite element analysis (FEA) was carried out to verify the stress concentration end areas of fracture. The interaction (etching time vs. surface treatment) was significant for Ra (p=0.008) and Rq (0.0075). Resin-treated groups presented significantly lower Ra and Rq than non-treated groups, except for the 60s group (p<0.005). SEM revealed that etching affected the ceramic microstructure and that the UR was able to penetrate into the irregularities. A significant effect of etching time (p=0.029) on flexural strength was seen. G7-G12 presented higher strength than G1-G6 (p<0.0001). None of experimental groups failed to show 95% confidence intervals of σ0 and m overlapped. FEA showed lower stress concentration after resin treatment. HF acid etching time did not show a damaging effect on the ceramic flexural strength. Moreover, the flexural strength could be enhanced after UR treatment. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Laboratory evaluation of the effect of unfilled resin after the use of self-etch and total-etch dentin adhesives on the Shear Bond Strength of composite to dentin.

PubMed

Nasseri, Ehsan Baradaran; Majidinia, Sara; Sharbaf, Davood Aghasizadeh

2017-05-01

Based on the frequent application of composite resins as tooth-colored fillings, this method is considered a viable alternative to dental amalgam. However, this method has the low bond strength of the composite to dentin. To solve this issue, various dental adhesive systems with different characteristics have been developed by dentistry experts. To assess the effect of an additional layer of unfilled resin in self-etch and total-etch dentin adhesives on the shear bond strength (SBS) of composite to dentin. Moreover, we assessed the effects of sample storage in artificial saliva on the SBS of composite to dentin. Methods: This experimental study was conducted on 160 freshly extracted human first or second premolar teeth, which were randomly divided into 16 groups. The teeth were prepared from Mashhad University of Medical Sciences, Mashhad, Iran (2008-2009). Scotchbond Multi-purpose (SBMP), single bond (SB), Clearfil SE Bond, and Clearfil S3 Bond were applied to dentin surface with or without the placement of hydrophobic resin (Margin Bond) in accordance with the instructions of the manufacturers. To expose the coronal dentin, the teeth were abraded with 600 grit SiC paper. Immediately after restoration, half of the samples were tested in terms of SBS, while the other samples were evaluated in terms of SBS after three months of storage in artificial saliva. SBS rates of dental composites evaluated by universal testing machine and samples were studied by optical stereomicroscopy to verify the failure type. Data analysis was performed in SPSS V.16 using Kolmogorov-Smirnov test, independent-samples t-test, ANOVA, and Duncan's logistic regression test. In this study, a significant reduction was observed in the SBS rates of SB and S3 bond adhesive systems after storage with and without hydrophobic resin (p>0.000). Without storage in normal saline, a significant increase was observed in the SBS rate of the SE bond (p=0.013). In addition, SBS rate of SBMP significantly increased after storage with hydrophobic resin (p=0.001). Finally, the highest and lowest rates of SBS were observed in the SE and S3 bonds in all the experimental groups, respectively. The effects of using a hydrophobic resin layer on shear bond strength values seem to be effective. The mild self-etch adhesive exhibited the best resin-dentine bond strength after aging.

Laboratory evaluation of the effect of unfilled resin after the use of self-etch and total-etch dentin adhesives on the Shear Bond Strength of composite to dentin

PubMed Central

Nasseri, Ehsan Baradaran; Majidinia, Sara; Sharbaf, Davood Aghasizadeh

2017-01-01

Background Based on the frequent application of composite resins as tooth-colored fillings, this method is considered a viable alternative to dental amalgam. However, this method has the low bond strength of the composite to dentin. To solve this issue, various dental adhesive systems with different characteristics have been developed by dentistry experts. Aim To assess the effect of an additional layer of unfilled resin in self-etch and total-etch dentin adhesives on the shear bond strength (SBS) of composite to dentin. Moreover, we assessed the effects of sample storage in artificial saliva on the SBS of composite to dentin. Methods Methods: This experimental study was conducted on 160 freshly extracted human first or second premolar teeth, which were randomly divided into 16 groups. The teeth were prepared from Mashhad University of Medical Sciences, Mashhad, Iran (2008–2009). Scotchbond Multi-purpose (SBMP), single bond (SB), Clearfil SE Bond, and Clearfil S3 Bond were applied to dentin surface with or without the placement of hydrophobic resin (Margin Bond) in accordance with the instructions of the manufacturers. To expose the coronal dentin, the teeth were abraded with 600 grit SiC paper. Immediately after restoration, half of the samples were tested in terms of SBS, while the other samples were evaluated in terms of SBS after three months of storage in artificial saliva. SBS rates of dental composites evaluated by universal testing machine and samples were studied by optical stereomicroscopy to verify the failure type. Data analysis was performed in SPSS V.16 using Kolmogorov-Smirnov test, independent-samples t-test, ANOVA, and Duncan’s logistic regression test. Results In this study, a significant reduction was observed in the SBS rates of SB and S3 bond adhesive systems after storage with and without hydrophobic resin (p>0.000). Without storage in normal saline, a significant increase was observed in the SBS rate of the SE bond (p=0.013). In addition, SBS rate of SBMP significantly increased after storage with hydrophobic resin (p=0.001). Finally, the highest and lowest rates of SBS were observed in the SE and S3 bonds in all the experimental groups, respectively. Conclusion The effects of using a hydrophobic resin layer on shear bond strength values seem to be effective. The mild self-etch adhesive exhibited the best resin-dentine bond strength after aging PMID:28713512

Shear Bond Strengths and Morphological Evaluation of Filled and Unfilled Adhesive Interfaces to Enamel and Dentine

PubMed Central

Mortazavi, Vajihesadat; Fathi, Mohammadhosein; Ataei, Ebrahim; Khodaeian, Niloufar; Askari, Navid

2012-01-01

In this laboratory study shear bond strengths of three filled and one unfilled adhesive systems to enamel and dentine were compared. Forty-eight extracted intact noncarious human mandibular molars were randomly assigned to two groups of 24 one for bonding to enamel and the other for bonding to dentine. Buccal and lingual surfaces of each tooth were randomly assigned for application of each one of filled (Prime & Bond NT (PBNT), Optibond Solo Plus (OBSP), and Clearfil SE Bond (CSEB)) and unfilled (Single Bond (SB)) adhesive systems (n = 12). A universal resin composite was placed into the translucent plastic cylinders (3 mm in diameter and 2 mm in length) and seated against the enamel and dentine surfaces and polymerized for 40 seconds. Shear bond strength was determined using a universal testing machine, and the results were statistically analyzed using two-way ANOVA, one-way ANOVA, t-test, and Tukey HSD post hoc test with a 5% level of significance.There were no statistically significant differences in bond strength between the adhesive systems in enamel, but CSEB and SB exhibited significantly higher and lower bond strength to dentine, respectively, than the other tested adhesive systems while there were no statistically significant differences between PBNT and OBSP. PMID:23209471

Addition Polyimides from Non-Mutagenic Diamines

NASA Technical Reports Server (NTRS)

Delvigs, Peter; Klopotek, David L.; Hardy-Green, DeNise; Meador, Michael A. (Technical Monitor)

2001-01-01

Studies were conducted to find an acceptable non-mutagenic diamine to replace 4,4'-methylenedianiline (MDA), a suspect carcinogen, which is currently being used in PMR-15 polyimide applications. Several diamines containing fluorine and trifluoromethyl substituent groups were synthesized. The diamines were polymerized with the dimethyl ester of 3,3',4,4'-benzophenone tetracarboxylic acid (BTDE), using the monomethyl ester of nadic acid (NE) as an endcap. The effect of diamine structure on rheological properties, glass transition temperature, and thermo-oxidative stability was investigated. Unidirectional laminates were fabricated from selected resins, using carbon fiber as the reinforcement. The results indicate that some of the diamines containing trifluoromethyl groups are non-mutagenic, and have potential to replace MDA in PMR polyimides for long-term applications at temperatures up to 300 C.

Development of lightweight graphite/polyimide sandwich panels.

NASA Technical Reports Server (NTRS)

Poesch, J. G.

1972-01-01

Lightweight graphite/polyimide composite honeycomb core and sandwich panels were fabricated and tested. Honeycomb cores of 1/4-in. and 3/8-in. cell sizes of hexagonal configuration were produced from thin plus or minus 45 deg cross plied sheets of prepreg producing core weights between 1.8 and 3.6 lb/cu ft. Thin gauge prepreg using Hercules graphite tow and Monsanto Skybond 710 polyimide resin were manufactured to produce cured ply thicknesses of 0.001 to 0.002 in. Graphite core properties measured at temperatures from -150 to 600 F are reported. Core properties which are superior to available materials were obtained. Sandwich panels weighing less than 0.5 lb/sq ft were designed and fabricated which meet the support structure loads for the shuttle orbiter thermal protection system.

RADIOLYTIC GAS PRODUCTION RATES OF POLYMERS EXPOSED TO TRITIUM GAS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Clark, E.

Data from previous reports on studies of polymers exposed to tritium gas is further analyzed to estimate rates of radiolytic gas production. Also, graphs of gas release during tritium exposure from ultrahigh molecular weight polyethylene (UHMW-PE), polytetrafluoroethylene (PTFE, a trade name is Teflon®), and Vespel® polyimide are re-plotted as moles of gas as a function of time, which is consistent with a later study of tritium effects on various formulations of the elastomer ethylene-propylene-diene monomer (EPDM). These gas production rate estimates may be useful while considering using these polymers in tritium processing systems. These rates are valid at least formore » the longest exposure times for each material, two years for UHMW-PE, PTFE, and Vespel®, and fourteen months for filled and unfilled EPDM. Note that the production “rate” for Vespel® is a quantity of H{sub 2} produced during a single exposure to tritium, independent of length of time. The larger production rate per unit mass for unfilled EPDM results from the lack of filler- the carbon black in filled EPDM does not produce H{sub 2} or HT. This is one aspect of how inert fillers reduce the effects of ionizing radiation on polymers.« less

Low-Cost Production of Composite Bushings for Jet Engine Applications

NASA Technical Reports Server (NTRS)

Gray, Robert A.

1998-01-01

The objectives of this research program were to reduce the manufacturing costs of variable stator vane bushings by 1) eliminating the expensive carbon fiber braiding operation, 2) replacing the batch mode impregnation, B-stage, and cutting operations with a continuous process, and 3) reducing the molding cycle and machining operations with injection molding to achieve near-net shapes. Braided bushings were successfully fabricated with both AMB-17XLD and AMB-TPD resin systems. The composite bushings achieved high glass transition temperature after post-cure (+300 C) and comparable weight loss to the PNM-15 bushings. ANM-17XLD bushings made with "batch-mode" molding compound (at 0.5 in. fiber length) achieved a +300 lb-force flange break strength which was superior to the continuous braided-fiber reinforced bushing. The non-MDA resin technology developed in this contract appears attractive for bushing applications that do not exceed a 300 C use temperature. Two thermoplastic polyimide resins were synthesized in order to generate injection molding compound powders. Excellent processing results were obtained at injection temperatures in excess of 300 C. Micro-tensile specimens were produced from each resin type and the Tg measurements (by TMA) for these samples were equivalent to AURUM(R). Thermal Gravimetric Analysis (TGA) conducted at 10 C/min showed that the non-MDA AMB-type polyimide thermoplastics had comparable weight loss to PMR-15 up to 500 C.

Evaluation of Double-Vacuum-Bag Process For Composite Fabrication

NASA Technical Reports Server (NTRS)

Hou, T. H.; Jensen, B. J.

2004-01-01

A non-autoclave vacuum bag process using atmospheric pressure alone that eliminates the need for external pressure normally supplied by an autoclave or a press is an attractive method for composite fabrication. This type of process does not require large capital expenditures for tooling and processing equipment. In the molding cycle (temperature/pressure profile) for a given composite system, the vacuum application point has to be carefully selected to achieve the final consolidated laminate net shape and resin content without excessive resin squeeze-out. The traditional single-vacuum- bag (SVB) process is best suited for molding epoxy matrix based composites because of their superior flow and the absence of reaction by-products or other volatiles. Other classes of materials, such as polyimides and phenolics, generate water during cure. In addition, these materials are commonly synthesized as oligomers using solvents to facilitate processability. Volatiles (solvents and reaction byproducts) management therefore becomes a critical issue. SVB molding, without additional pressure, normally fails to yield void-free quality composites for these classes of resin systems. A double-vacuum- bag (DVB) process for volatile management was envisioned, designed and built at the NASA Langley Research Center. This experimental DVB process affords superior volatiles management compared to the traditional SVB process. Void-free composites are consistently fabricated as measured by C-scan and optical photomicroscopy for high performance polyimide and phenolic resins.

Thermal Cycling of Thermal Control Paints on Carbon-Carbon and Carbon-Polyimide Composites

NASA Technical Reports Server (NTRS)

Jaworske, Donald A.

2006-01-01

Carbon-carbon composites and carbon-polyimide composites are being considered for space radiator applications owing to their light weight and high thermal conductivity. For those radiator applications where sunlight will impinge on the surface, it will be necessary to apply a white thermal control paint to minimize solar absorptance and enhance infrared emittance. Several currently available white thermal control paints were applied to candidate carbon-carbon and carbon-polyimide composites and were subjected to vacuum thermal cycling in the range of -100 C to +277 C. The optical properties of solar absorptance and infrared emittance were evaluated before and after thermal cycling. In addition, adhesion of the paints was evaluated utilizing a tape test. The test matrix included three composites: resin-derived carbon-carbon and vapor infiltrated carbon-carbon, both reinforced with pitch-based P-120 graphite fibers, and a polyimide composite reinforced with T-650 carbon fibers, and three commercially available white thermal control paints: AZ-93, Z-93-C55, and YB-71P.

Degradation of strength properties of epoxy resin filled with natural-based particles

NASA Astrophysics Data System (ADS)

Valášek, Petr; Habrová, Karolína; Müller, Miroslav

2018-05-01

Degradation of polymeric materials can be considered as a limiting factor for their use. Mechanical characteristics of epoxy resins are reduced, for example, by the action and changes of temperature or humidity. Degradation also occurs in composite systems where the epoxy resins function as matrices, i.e. in polymer composite materials. If a natural filler is used together with the epoxy resin, we refer to these materials as biocomposites, where also the natural character of the filler material greatly affects the degradation process. The paper focuses on the description of the shear strength of the resin filled with particles prepared from the seeds of dates of Phoenix Dactylifera plant. The degradation was evaluated experimentally in laboratory conditions via the climatic chamber. The experiment describes composites with a particle size of filler 100-200 μm with a concentration of 5 - 10 wt%. As the number of degradation cycles increased, the tensile strength of both the unfilled and the filled epoxy resin decreased. After 5 weeks, the drop was up to 50%. The presence of the particles did not significantly affect the shear strength compared to the non-filled resin. The described way of utilization of the natural-based particles is the possibility of material utilization of secondary natural materials.

Preparation for foam composites. [using polybenzimidazole for fireproofing panels

NASA Technical Reports Server (NTRS)

Maximovich, M. G.

1974-01-01

Methods were developed for the fabrication of fire resistant panels utilizing polybenzimidazole (PBI) and Kerimid 601 resins along with glass, quartz, and Kevlar reinforcements. Stitched truss structure, both unfilled and filled with PBI foam, were successfully fabricated and tested. Second generation structures were then selected, fabricated, and tested, with a PBI/glass skin/PBI foam sandwich structure emerging as the optimum panel concept. Mechanical properties, smoke generation, and fire resistance were determined for the candidate panels.

Development of critical molecular weight-property specifications for high performance polymers used as adhesives and composites

NASA Technical Reports Server (NTRS)

Kranbuehl, D. E.

1982-01-01

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.

Zinc incorporation improves biological activity of beta-tricalcium silicate resin-based cement.

PubMed

Osorio, Raquel; Yamauti, Monica; Sauro, Salvatore; Watson, Tim F; Toledano, Manuel

2014-11-01

Matrix metalloproteinase (MMP) inhibition may improve endodontic treatment prognosis. The purpose of this study was to determine if zinc incorporation into experimental resin cements containing bioactive fillers may modulate MMP-mediated collagen degradation of dentin. Human dentin samples untreated and demineralized using 10% phosphoric acid or 0.5 mol/L EDTA were infiltrated with the following experimental resins: (1) unfilled resin, (2) resin with Bioglass 45S5 particles (OSspray, London, UK), (3) resin with beta-tricalcium silicate particles (βTCS), (4) resin with zinc-doped Bioglass 45S5, and (5) resin with zinc-doped βTCS particles. The specimens were stored in artificial saliva (for 24 hours, 1 week, and 4 weeks) and submitted to radioimmunoassay to quantify C-terminal telopeptide. Scanning electron microscopy analysis was also undertaken on dentin samples after 4 weeks of storage. Collagen degradation was prominent both in phosphoric acid and EDTA-treated dentin. Resin infiltration strongly reduced MMP activity in demineralized dentin. Resin containing Bioglass 45S5 particles exerted higher and stable protection of collagen. The presence of zinc in βTCS particles increases MMP inhibition. Different mineral precipitation was attained in dentin infiltrated with the resin cements containing bioactive fillers. MMP degradation of dentin collagen is strongly reduced after resin infiltration of dentin. Zinc incorporation in βTCS particles exerted an additional protection against MMP-mediated collagen degradation. However, it did not occur in resin containing Bioglass 45S5 particles, probably because of the formation of phosphate-zinc compounds. Copyright © 2014 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

Mechanical and electrical properties of laminates for high performance printed wiring boards

NASA Astrophysics Data System (ADS)

Guiles, Chester L.

The physical and electrical properties of laminate boards intended for high-performance applications are reviewed with particular reference to the coefficient of thermal expansion, dielectric constant, and characteristic impedance. It is shown, in particular, that the electrical properties can be tailored to some extent by using various conbinations of basic board materials, such as copper foil, fiberglass fabric, glass fabric, epoxy resin, polyimide resin, aluminum sheet, Kevlar and quartz fabrics, copper-invar-copper, and alumina-ceramic.

Polymer Infiltration Studies

NASA Technical Reports Server (NTRS)

Marchello, Joseph M.

1991-01-01

Progress was made on the preparation of carbon fiber composites using advanced polymer resins. Processes reported include powder towpreg process, weaving towpreg made from dry powder prepreg, composite from powder coated towpreg, and toughening of polyimide resin (PMR) composites by semi-interpenetrating networks. Several important areas of polymer infiltration into fiber bundles will be researched. Preparation to towpreg for textile preform weaving and braiding and for automated tow placement is a major goal, as are the continued development of prepregging technology and the various aspects of composite part fabrication.

Toughening of PMR composites by gradient semi-interpenetrating networks

NASA Technical Reports Server (NTRS)

Johnston, N. J.; Srinivasan, K.; Peter, R. H.

1992-01-01

The toughening of the PMR-15 and LARC RP-46 high temperature thermosetting polyimides is presently attempted through the construction of a semiinterpenetrating network at ply interfaces through the use of the Matrimid 5218 thermoplastic polyimide powder, whose 315-320 glass transition temperature is compatible with the PMR matrices. The 60 vol pct fiber composites thus prepared for the two resins, with and without toughening, were comprehensively characterized in flexure, tension, intralaminar and short beam shear, compression and quasi-isotropic short-block compression, as well as modes I and II interlaminar fracture toughness and compression after impact.

Hollow Polyimide Microspheres

NASA Technical Reports Server (NTRS)

Weiser, Erik S. (Inventor); St.Clair, Terry L. (Inventor); Echigo, Yoshiaki (Inventor); Kaneshiro, Hisayasu (Inventor)

1999-01-01

A shaped article composed of an aromatic polyimide has a hollow, essentially spherical structure and a particle size of about 100 to about 1500 microns, a density of about I to about 6 pounds/ft3 and a volume change of 1 to about 20% by a pressure treatment of 30 psi for 10 minutes at room temperature. A syntactic foam, made of a multiplicity of the shaped articles which are bounded together by a matrix resin to form an integral composite structure, has a density of about 3 to about 30 pounds/cu ft and a compression strength of about 100 to about 1400 pounds/sq in.

Hollow Polyimide Microspheres

NASA Technical Reports Server (NTRS)

Weiser, Erik S. (Inventor); St.Clair, Terry L. (Inventor); Echigo, Yoshiaki (Inventor); Kaneshiro, Hisayasu (Inventor)

2001-01-01

A shaped article composed of an aromatic polyimide has a hollow, essentially spherical structure and a particle size of about 100 to about 1500 micrometers, a density of about 1 to about 6 pounds/cubic foot and a volume change of 1 to about 20% by a pressure treatment of 30 psi for 10 minutes at room temperature. A syntactic foam, made of a multiplicity of the shaped articles which are bonded together by a matrix resin to form an integral composite structure, has a density of about 3 to about 30 pounds/cubic feet and a compression strength of about 100 to about 1400 pounds/sq inch.

Resin Transfer Moldable Polyimides Developed for High-Temperature Applications

NASA Technical Reports Server (NTRS)

Meador, Mary Ann

2000-01-01

High-temperature polyimides, such as PMR 15 (which was developed at the NASA Glenn Research Center at Lewis Field), are becoming an increasingly important class of materials for a variety of aerospace applications, such as aircraft engine components and propulsion and airframe components for reusable launch vehicles (RLV s). Because of their high specific strength and low density, use of these materials in place of more traditional aerospace materials, such as titanium, can significantly reduce component and vehicle weight, leading to reductions in fuel consumption (and pollutants), increases in payload and passenger capacity, and improvements in vehicle performance.

Development of a protective decorative fire resistant low smoke emitting, thermally stable coating material

NASA Technical Reports Server (NTRS)

1976-01-01

The development of suitable electrocoatings and subsequent application to nonconductive substrates are discussed. Substrates investigated were plastics or resin-treated materials such as FX-resin (phenolic-type resin) impregnated fiberglass mat, polyphenylene sulfide, polyether sulfone and polyimide-impregnated unidirectional fiberglass. Efforts were aimed at formulating a fire-resistant, low smoke emitting, thermally stable, easily cleaned coating material. The coating is to be used for covering substrate panels, such as aluminum, silicate foam, polymeric structural entities, etc., all of which are applied in the aircraft cabin interior and thus subject to the spillages, scuffing, spotting and the general contaminants which prevail in aircraft passenger compartments.

Low-Melt Polyamic Acid Based Powder Coatings

NASA Technical Reports Server (NTRS)

Jolley, Scott T. (Inventor)

2017-01-01

The present invention is directed to a method for powder coating a metal substrate using a low-melt polyamic acid (PAA) polymer that readily imidizes to polyimides. These low-melt PAAs have been shown to be useful in resins applied as powder coatings to metal surfaces. The resin includes an end-capping material capable of providing crosslinking functionality to at least one end of the low-melt PAA polymer. The end-capping material functions dually as a polymerization chain terminator and crosslinking agent, thus producing resins that have molecular weights low enough to flow well and form good cured films applicable for use in powder coating.

Rapid viscosity measurements of powdered thermosetting resins

NASA Technical Reports Server (NTRS)

Price, H. L.; Burks, H. D.; Dalal, S. K.

1978-01-01

A rapid and inexpensive method of obtaining processing-related data on powdered thermosetting resins has been investigated. The method involved viscosity measurements obtained with a small specimen (less than 100 mg) parallel plate plastometer. A data acquisition and reduction system was developed which provided a value of viscosity and strain rate about 12-13 second intervals during a test. The effects of specimen compaction pressure and reduction of adhesion between specimen and parallel plates were examined. The plastometer was used to measure some processing-related viscosity changes of an addition polyimide resin, including changes caused by pre-test heat treatment, test temperature, and strain rate.

FTIR Monitoring Of Curing Of Composites

NASA Technical Reports Server (NTRS)

Druy, Mark A.; Stevenson, William A.; Young, Philip R.

1990-01-01

Infrared-sensing optical fiber system developed to monitor principal infrared absorption bands resulting from vibrations of atoms and molecules as chemical bonds form when resin cured. System monitors resin chemistry more directly. Used to obtain Fourier transform infrared (FTIR) spectrum from graphite fiber/polyimide matrix resin prepreg. Embedded fiber optic FTIR sensor used to indicate state of cure of thermosetting composite material. Developed primarily to improve quality of advanced composites, many additional potential applications exist because principal of operation applicable to all organic materials and most inorganic gases. Includes monitoring integrities of composite materials in service, remote sensing of hazardous materials, and examination of processes in industrial reactors and furnaces.

The development of autoclave processable, thermally stable adhesives for titanium alloy and graphite composite structures

NASA Technical Reports Server (NTRS)

Vaughan, R. W.; Jones, R. J.

1971-01-01

The A-type polyimide adhesive resin P11B was modified by use of mixed diamines (thio-dianiline and meta phenylene diamine) which provided the desired autoclave processability. This new resin was termed P11BA. It was shown that copolymeric blends of P11BA and Amoco AI-1137 amide-imide resin provided improved adhesive properties when autoclave processed over the properties obtained previously by press bonding with P11B based copolymeric blended adhesives. Properties of bonded assemblies are presented for long-term aging at both elevated and low temperatures, and also stress-rupture tests at elevated temperature.

Effects of thermal and environmental exposure on the mechanical properties of graphite/polyimide composites

NASA Technical Reports Server (NTRS)

Hanson, M. P.; Serafini, T. T.

1971-01-01

Composites were exposed in circulating and static air environments up to 589 K for a maximum of 1000 hours. Composites of HT-S, HM-S, Thornel 50S, and Fortafil 5-Y fiber and a new addition type polyimide resin were laminated in a matched-die mold. Flexural strengths, flexural modulus, and interlaminar shear strengths were determined at 297, 533, and 598 K after various durations of exposure. Composite and fiber weight loss characteristics were determined by isothermal gravimetric analysis in air. Properties of composites exposed and tested at the environment temperatures were compared with those determined under short-term exposure. A new short beam interlaminar shear fixture is described. Environmental effects of long-term ambient temperature exposure on the elevated temperature mechanical properties of graphite/polyimide composites are presented.

V-378A: A modified bismaleimide for advanced composites

NASA Technical Reports Server (NTRS)

Street, S. W.

1985-01-01

Addition polyimides cure with no evolution of gaseous by-products at relatively low temperatures and may be cured at low pressures to yield composites with excellent hot-wet strength retention. These properaties have made them excellent candidates as matrix resins for advanced composites. However, commercially available bismaleimides are solids and difficult to handle in preimpregnated form. V-378A is an addition polyimide composed of a mixture of bismaleimides and other reactive ingredients formulated to provide good prepreg properties and handling, facile cure and excellent composite mechanical properties. Several curing mechanisms are utilized to provide the characteristics exhibited by V-378A. Part of the mechanism is free radial and takes place at ambient temperature and above. Other mechanisms are principally Diels-Alder in nature. V-378A prepregs are tacky at ambient temperature, but do not have long tacky outlife similar to some epoxies. V-378A yields composites which exhibit hot-wet strength retention which is superior to that provided by epoxy resin systems.

Platelet composite coatings for tin whisker mitigation

DOE PAGES

Rohwer, Lauren E. S.; Martin, James E.

2015-09-14

In this study, reliable methods for tin whisker mitigation are needed for applications that utilize tin-plated commercial components. Tin can grow whiskers that can lead to electrical shorting, possibly causing critical systems to fail catastrophically. The mechanisms of tin whisker growth are unclear and this makes prediction of the lifetimes of critical components uncertain. The development of robust methods for tin whisker mitigation is currently the best approach to eliminating the risk of shorting. Current mitigation methods are based on unfilled polymer coatings that are not impenetrable to tin whiskers. In this paper we report tin whisker mitigation results formore » several filled polymer coatings. The whisker-penetration resistance of the coatings was evaluated at elevated temperature and high humidity and under temperature cycling conditions. The composite coatings comprised Ni and MgF 2-coated Al/Ni/Al platelets in epoxy resin or silicone rubber. In addition to improved whisker mitigation, these platelet composites have enhanced thermal conductivity and dielectric constant compared with unfilled polymers.« less

Platelet Composite Coatings for Tin Whisker Mitigation

NASA Astrophysics Data System (ADS)

Rohwer, Lauren E. S.; Martin, James E.

2015-11-01

Reliable methods for tin whisker mitigation are needed for applications that utilize tin-plated commercial components. Tin can grow whiskers that can lead to electrical shorting, possibly causing critical systems to fail catastrophically. The mechanisms of tin whisker growth are unclear and this makes prediction of the lifetimes of critical components uncertain. The development of robust methods for tin whisker mitigation is currently the best approach to eliminating the risk of shorting. Current mitigation methods are based on unfilled polymer coatings that are not impenetrable to tin whiskers. In this paper we report tin whisker mitigation results for several filled polymer coatings. The whisker-penetration resistance of the coatings was evaluated at elevated temperature and high humidity and under temperature cycling conditions. The composite coatings comprised Ni and MgF2-coated Al/Ni/Al platelets in epoxy resin or silicone rubber. In addition to improved whisker mitigation, these platelet composites have enhanced thermal conductivity and dielectric constant compared with unfilled polymers.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rohwer, Lauren E. S.; Martin, James E.

In this study, reliable methods for tin whisker mitigation are needed for applications that utilize tin-plated commercial components. Tin can grow whiskers that can lead to electrical shorting, possibly causing critical systems to fail catastrophically. The mechanisms of tin whisker growth are unclear and this makes prediction of the lifetimes of critical components uncertain. The development of robust methods for tin whisker mitigation is currently the best approach to eliminating the risk of shorting. Current mitigation methods are based on unfilled polymer coatings that are not impenetrable to tin whiskers. In this paper we report tin whisker mitigation results formore » several filled polymer coatings. The whisker-penetration resistance of the coatings was evaluated at elevated temperature and high humidity and under temperature cycling conditions. The composite coatings comprised Ni and MgF 2-coated Al/Ni/Al platelets in epoxy resin or silicone rubber. In addition to improved whisker mitigation, these platelet composites have enhanced thermal conductivity and dielectric constant compared with unfilled polymers.« less

The 371 deg C mechanical properties of graphite/polyimide composites

NASA Technical Reports Server (NTRS)

Delvigs, P.

1985-01-01

A series of condensation polyimides based on pyromellitic dianhydride is synthesized and evaluated for potential application at 371 C. Several three-and four-ring benzenoid diamine systems containing oxygen bridging groups are investigated. Thermomechanical analysis of neat resin specimens indicate that the polyimide prepared from the dimethyl ester of pyrometallitic acid (PMDE) and 2,2-bis4-(4'-aminophenoxy) phenyl]-1,1,1,3,3,3- hexafluoropropane (BDAF) is the only resin system which has a glass transition temperature (Tg) above 371 C. The Tg of the PMDE/BDAF polyimide is found to be 390 C after a postcure air at 371 C for 24 hr. Unidirectional composites are fabricated from the PMDE/BDAF system and unsized Celion 6000 graphite fibers. Final cure temperatures in the range of 371 to 427 C with an applied pressure of 10.34 to 13.78 MPa are investigated. The void content of the composites ranges from 4.6 to 8.6 percent. Composites cured at 399 C under a pressure of 10.34 MPa and postcured in air at 371 C for 24 hr exhibit the highest 371 C interlaminar shear strength (ILSS, 40.7 MPa) and flexural strength (758 MPa). The thermo-oxidative stability of the composites is determined by subjecting specimens to isothermal exposure at 371 C in air at atmospheric pressure, as well as a pressure of 0.52 MPa. Specimens exposed at atmospheric pressure exhibit a weight loss of 12 percent after 200 hr of exposure and 88 percent retention of its original 371 C ILSS. In contrast, the specimens exposed at 0.52 MPa pressure exhibit a comparable weight loss after only 72 hr, and a 71 percent retention of its original 371 C ILSS.

Properties of M40J Carbon/PMR-II-50 Composites Fabricated with Desized and Surface Treated Fibers. Characterization of M40J Desized and Finished Fibers

NASA Technical Reports Server (NTRS)

Allred, Ronald E.; Gosau, Jan M.; Shin, E. Eugene; McCorkle, Linda S.; Sutter, James K.; OMalley, Michelle; Gray, Hugh R. (Technical Monitor)

2002-01-01

To increase performance and durability of high temperature composites for potential rocket engine components, it is necessary to optimize wetting and interfacial bonding between high modulus carbon fibers and high temperature polyimide resins. It has been previously demonstrated that the electro-oxidative shear treatments used by fiber manufacturers are not effective on higher modulus fibers that have fewer edge and defect sites in the surface crystallites. In addition, sizings commercially supplied on most carbon fibers are not compatible with polyimides. This study was an extension of prior work characterizing the surface chemistry and energy of high modulus carbon fibers (M40J and M60J, Torray) with typical fluorinated polyimide resins, such as PMR-II-50. A continuous desizing system which utilizes environmentally friendly chemical- mechanical processes was developed for tow level fiber and the processes were optimized based on weight loss behavior, surface elemental composition (XPS) and morphology (FE-SEM) analyses, and residual tow strength of the fiber, and the similar approaches have been applied on carbon fabrics. Both desized and further treated with a reactive finish were investigated for the composite reinforcement. The effects of desizing and/or subsequent surface retreatment on carbon fiber on composite properties and performance including fiber-matrix interfacial mechanical properties, thermal properties and blistering onset behavior will be discussed in this presentation.

Experimental resin cements containing bioactive fillers reduce matrix metalloproteinase-mediated dentin collagen degradation.

PubMed

Osorio, Raquel; Yamauti, Monica; Sauro, Salvatore; Watson, Thimoty F; Toledano, Manuel

2012-09-01

Collagen dentin matrix may represent a suitable scaffold to be remineralized in the presence of bioactive materials. The purpose of this study was to determine if experimental resin cements containing bioactive fillers may modulate matrix metalloproteinase-mediated collagen degradation of etched dentin. Human dentin beams demineralized using 10% phosphoric acid or 0.5 mol/L EDTA were infiltrated with the following experimental resins: (1) unfilled resin, (2) resin with Bioglass 45S5 particles (Sylc; OSspray Ltd, London, UK), and (3) resin with β-tricalcium phosphate-modified calcium silicate cement (HCAT-β) particles. The filler/resin ratio was 40/60 wt%. The specimens were stored in artificial saliva, and the determination of C-terminal telopeptide (ICTP) was performed by radioimmunoassay after 24 hours, 1 week, and 4 weeks. Scanning electron microscopic analysis of dentin surfaces after 4 weeks of storage was also executed. Collagen degradation was prominent both in phosphoric acid and EDTA-treated dentin. Resin infiltration strongly reduced the MMP activity in demineralized dentin. Resin-containing Bioglass 45S5 particles exerted higher and more stable protection of collagen at all tested dentin states and time points. HCAT-β induced collagen protection from MMPs only in EDTA-treated specimens. Dentin remineralization was achieved when dentin was infiltrated with the resin cements containing bioactive fillers. MMP degradation of dentin collagen is strongly reduced in resin-infiltrated dentin. The inclusion of Bioglass 45S5 particles exerted an additional protection of collagen during dentin remineralization. Copyright © 2012 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

Silicone modified resins for graphite fiber laminates

NASA Technical Reports Server (NTRS)

Frost, L. W.; Bower, G. M.

1979-01-01

The development of silicon modified resins for graphite fiber laminates which will prevent the dispersal of graphite fibers when the composites are burned is discussed. Eighty-five silicone modified resins were synthesized and evaluated including unsaturated polyesters, thermosetting methacrylates, epoxies, polyimides, and phenolics. Neat resins were judged in terms of Si content, homogeneity, hardness, Char formation, and thermal stability. Char formation was estimated by thermogravimetry to 1,000 C in air and in N2. Thermal stability was evaluated by isothermal weight loss measurements for 200 hrs in air at three temperatures. Four silicone modified epoxies were selected for evaluation in unidirectional filament wound graphite laminates. Neat samples of these resins had 1,000 C char residues of 25 to 50%. The highest flexural values measured for the laminates were a strength of 140 kpsi and a modulus of 10 Mpsi. The highest interlaminar shear strength was 5.3 kpsi.

Second generation PMR polyimide/fiber composites

NASA Technical Reports Server (NTRS)

Cavano, P. J.

1979-01-01

A second generation polymerization monomeric reactants (PMR) polyimdes matrix system (PMR 2) was characterized in both neat resin and composite form with two different graphite fiber reinforcements. Three different formulated molecular weight levels of laboratory prepared PMR 2 were examined, in addition to a purchased experimental fully formulated PMR 2 precurser solution. Isothermal aging of graphite fibers, neat resin samples and composite specimens in air at 316 C were investigated. Humidity exposures at 65 C and 97 percent relative humidity were conducted for both neat resin and composites for eight day periods. Anaerobic char of neat resin and fire testing of composites were conducted with PMR 15, PMR 2, and an epoxy system. Composites were fire tested on a burner rig developed for this program. Results indicate that neat PMR 2 resins exhibit excellent isothermal resistance and that PMR 2 composite properties appear to be influenced by the thermo-oxidative stability of the reinforcing fiber.

Polyimide Composites Properties of RTM370 Fabricated by Vacuum Assisted Resins Transfer Molding (VARTM)

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.; Criss, Jim M.; Mintz, Eric A.

2011-01-01

RTM370 imide resin based on 2,3,3 ,4 -biphenyl dianhydride ( a-BPDA), 3,4 -oxydianinline (3,4 -ODA) with 4-phenylethynylphthalic (PEPA) endcap has shown to exhibit high Tg (370 C) and low melt viscosity (10-30 poise) at 280 C with a pot-life of 1-2 h. Previously, RTM370 resin has been fabricated into composites with T650-35 carbon fabrics by resin transfer molding (RTM) successfully. RTM370 composites exhibit excellent mechanical properties up to 327 C (620 F), and outstanding property retention after aging at 288 C (550 F) for 1000 hrs. In this presentation, RTM 370 composites will be fabricated by vacuum assisted resins transfer molding (VARTM), using vacuum bags without mold. The mechanical properties of RTM370 composites fabricated by VARTM will be compared to those of RTM370 made by RTM.

Composite Properties of RTM370 Polyimide Fabricated by Vacuum Assisted Resin Transfer Molding (VARTM)

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.; Criss, James M.; Mintz, Eric A.; Shonkwiler, Brian; McCorkle, Linda S.

2011-01-01

RTM370 imide resin based on 2,3,3?,4?-biphenyl dianhydride (a-BPDA), 3,4'-oxydianinline (3,4'-ODA) with the 4-phenylethynylphthalic (PEPA) endcap has been shown to exhibit a high cured T(sub g) (370 C) and low melt viscosity (10-30 poise) at 280 C with a pot-life of 1-2 h. Previously, RTM370 resin has been successfully fabricated into composites reinforced with T650-35 carbon fabrics by resin transfer molding (RTM). RTM370 composites exhibit excellent mechanical properties up to 327?C (620?F), and outstanding property retention after aging at 288?C (550?F) for 1000 h. In this work, RTM370 composites were fabricated by vacuum assisted resin transfer molding (VARTM), using vacuum bags on a steel plate. The mechanical properties of RTM370 composites fabricated by VARTM are compared to those prepared by RTM.

Improving processing and toughness of a high performance composite matrix through an interpenetrating polymer network. VI

NASA Technical Reports Server (NTRS)

Pater, Ruth H.

1990-01-01

A simultaneous semi-interpenetrating polymer network (semi-IPN) concept is presented which combines easy-to-process, but brittle, thermosetting polyimides with tough, but difficult to process, linear thermoplastic polyimides. The combination results in a semi-IPN with the easy processability of a thermoset and good toughness of a thermoplastic. Four simultaneous semi-IPN systems were developed from commercially available NR-150B2 combined with each of the four Thermid materials (LR-600, AL-600, MC-600, and FA-700). It is concluded that there is a significant improvement in resin fracture toughness of Thermid-polyimide-based semi-IPN systems and some improvement in composite microcracking resistance compared to Thermid LR-600. Excellent composite mechanical properties have been achieved. These new semi-IPN materials have the potential to be used as composite matrices, adhesives, and molding materials.

NR-150B2 adhesive development

NASA Technical Reports Server (NTRS)

Blatz, P. S.

1978-01-01

Adhesive based polyimide solutions which are more easily processed than conventional aromatic polyimide systems and show potential for use for extended times at 589K are discussed. The adhesive system is based on a solution containing diglyme as the solvent and 2,2 bis(3',4'-dicarboxyphenyl)hexafluoropropane, paraphenylenediamine, and oxydianiline. The replacement of N-methylpyrrolidone with diglyme as the solvent was found to improve the adhesive strengths of lap shear samples and simplify the processing conditions for bonding both titanium and graphite fiber/polyimide matrix resin composites. Information was obtained on the effects of various environments including high humidity, immersion in jet fuel and methylethylketone on aluminum filled adhesive bonds. The adhesive was also evaluated in wide area bonds and flatwise tensile specimens using titanium honeycomb and composite face sheets. It was indicated that the developed adhesive system has the potential for use in applications requiring long term exposure to at least 589K (600 F).

Out of the Autoclave Fabrication of LaRC[TradeMark] PETI-9 Polyimide Laminates

NASA Technical Reports Server (NTRS)

Cano, Robert J.; Jensen, Brian J.

2013-01-01

The NASA Langley Research Center developed polyimide system, LaRC PETI-9, has successfully been processed into composites by high temperature vacuum assisted resin transfer molding (HT-VARTM). To extend the application of this high use temperature material to other out-of-autoclave (OOA) processing techniques, the fabrication of PETI- 9 laminates was evaluated using only a vacuum bag and oven cure. A LaRC PETI-9 polyimide solution in NMP was prepared and successfully utilized to fabricate unidirectional IM7 carbon fiber prepreg that was subsequently processed into composites with a vacuum bag and oven cure OOA process. Composite panels of good quality were successfully fabricated and mechanically tested. Processing characteristics, composite panel quality and mechanical properties are presented in this work. The resultant properties are compared to previously developed LaRC material systems processed by both autoclave and OOA techniques including the well characterized, autoclave processed LaRC PETI-5.

The effect on the flexural strength, flexural modulus and compressive strength of fibre reinforced acrylic with that of plain unfilled acrylic resin - an in vitro study.

PubMed

Thomas, Tony C; K, Aswini Kumar; Mohamed, Shamaz; Krishnan, Vinod; Mathew, Anil; V, Manju

2015-03-01

The aim of this in vitro study was to compare the flexural strength, the flexural modulus and compressive strength of the acrylic polymer reinforced with glass, carbon, polyethylene and Kevlar fibres with that of plain unfilled resin. A total of 50 specimens were prepared and divided into 10 specimens each under 5 groups namely group 1- control group without any fibres, group 2 - carbon fibres, group 3- glass fibres, group 4 - polyethylene, group 5- Kevlar. Universal testing machine (Tinius olsen, USA) was used for the testing of these specimens. Out of each group, 5 specimens were randomly selected and testing was done for flexural strength using a three point deflection test and three point bending test for compressive strength and the modulus was plotted using a graphical method. Statistical analysis was done using statistical software. The respective mean values for samples in regard to their flexural strength for PMMA plain, PMMA+ glass fibre, PMMA+ carbon, PMMA+ polyethylene and PMMA+ Kevlar were 90.64, 100.79, 102.58, 94.13 and 96.43 respectively. Scheffes post hoc test clearly indicated that only mean flexural strength values of PMMA + Carbon, has the highest mean value. One-way ANOVA revealed a non-significant difference among the groups in regard to their compressive strength. The study concludes that carbon fibre reinforced samples has the greatest flexural strength and greatest flexural modulus, however the compressive strength remains unchanged.

Experiments Related to the Fabrication of Carbon Fiber/AMB-21 Polyimide Composite Tubes Using the RTM Process

NASA Technical Reports Server (NTRS)

Exum, Daniel

1996-01-01

AMB-21 is a new polymer developed by Mr. Ray Vannucci, NASA, LeRC as a noncarcinogenic polyimide matrix which may be suitable for fabricating composite parts by the Resin Transfer Modeling (RTM) process. The polyimide for this project was prepared at the Center of Composite Materials Research at N.C. A&T State University because it is not currently an item of commerce. The RTM process is especially suitable for producing geometrically complex composite parts at a low cost. Because of the high melting point and very high viscosity at the time of processing, polyimides have not been extensively used in the RTM process. The process for preparing AMB-21 as well as the process for fabricating composite plates will be described. The basic fabrication process consists of injecting a solvent solution of AMP-21 into a carbon fiber preform, evaporating the solvent, imidizing the polyimide, and vacuum/compression modeling the impregnated preform. All the above molding steps are preformed in a specially designed RTM mold which will be described. The results of this process have been inconsistent. Where as some experiments have resulted in a reasonably sound panels, others have not. Further refinements of the process are required to establish a reliable process.

Fabrication and Evaluation of Graphite Fiber-Reinforced Polyimide Composite Tube Forms Using Modified Resin Transfer Molding

NASA Technical Reports Server (NTRS)

Exum, Daniel B.; Ilias, S.; Avva, V. S.; Sadler, Bob

1997-01-01

The techniques necessary for the fabrication of a complex three-dimensional tubular form using a PMR-type resin have been developed to allow for the construction of several tubes with good physical and mechanical properties. Employing established resin transfer molding practices, the relatively non-hazardous AMB-21 in acetone formulation was used to successfully impregnate four layers of AS4 braided graphite fiber preform previously loaded around an aluminum cylindrical core in an enclosed mold cavity. Using heat and vacuum, the solvent was evaporated to form a prepreg followed by a partial imidization and removal of condensation products. The aluminum core was replaced by a silicone rubber bladder and the cure cycle continued to the final stage of 550 F with a bladder internal pressure of 200 lbs/sq in while simultaneously applying a strong vacuum to the prepreg for removal of any additional imidization products. A combination of several modifications to the standard resin transfer molding methodology enabled the mold to 'breathe', allowing the imidization products a pathway for escape. AMB-21 resin was chosen because of the carcinogenic nature of the primary commercial polyimide PMR-15. The AMB-21 resin was formulated using commercially available monomers or monomer precursors and dissolved in a mixture of methyl alcohol and acetone. The viscosity of the resulting monomer solution was checked by use of a Brookfield rheometer and adjusted by adding acetone to an easily pumpable viscosity of about 600 cP. In addition, several types of chromatographic and thermal analyses were of the braids, and excess handling of the preforms broke some of the microscopic fibers, needlessly decreasing the strength of the finished part. In addition, three dimensional braided preforms with fibers along the length of the tube will be significantly stronger in tension than the braided preforms used in this study.

New processable modified polyimide resins for adhesive and matrix applications

NASA Technical Reports Server (NTRS)

Landman, D.

1985-01-01

A broad product line of bismaleimide modified epoxy adhesives which are cured by conventional addition curing methods is described. These products fill a market need for 232 C (450 F) service adhesives which are cured in a manner similar to conventional 177 C (350 F) epoxy adhesives. The products described include film adhesives, pastes, and a primer. Subsequent development work has resulted in a new bismaleimide modified epoxy resin which uses a unique addition curing mechanism. This has resulted in products with improved thermomechanical properties compared to conventional bismaleimide epoxy resins. A film adhesive, paste, and matrix resin for composites using this new technology are described. In all cases, the products developed are heat cured by using typical epoxy cure cycles i.e., 1 hour at 177 C (350 F) followed by 2 hours postcure at 246 C (475 F).

Polyimides containing oxyethylene units. Part 4: Polymerization of dianhydrides containing ether linkages

NASA Technical Reports Server (NTRS)

Harris, F. W.; Karnavas, A. J.; Das, S.; Cucuras, C. N.; Hergenrother, P. M.

1986-01-01

The development of new composite resins for various aerospace applications is attempted. Although it is highly desirable that these polymers be soluble in order to facilitate processing, they must display considerable solvent-resistance in use. A recent approach has involved the synthesis of a new series of polyimides containing flexible linkages. The polymers were prepared by the polymerization of aromatic dianhydrides with diamines containing oxyethylene linkages. For example, the polymerization of 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA) with 1,2-bis(4-aminophenoxy)ethane (1a) and bis2-(4-aminophenoxy)ethylether (lb), afforded highly crystalline polyimides that were completely insoluble. However, a polyimide that was amorphous and soluble was obtained from the polymerization of BTDA and an isomer of lb, i.e., bis2-(3-aminophenoxy)ethyl ether (4b). In an attempt to obtain a soluble, amorphous polyimide that could be annealed into a crysalline state, block copolymers of 1b and 4b and BTDA were prepared. Copolymers containing less than 20 weight % 1b were soluble in organic solvents. However, these polymers did not crystallize when heated above their Tg's. Copolymers containing higher levels of 1b were semicrystalline and insoluble. The polymerization of the diamines containing oxyethylene linkages with 4,4'-oxydiphthalic anhydride (ODPA) and a new dianhydride, i.e., 4,4'-oxyethyleneoxyethyleneoxydiphthalic anhydride (OEDA) was investigated. It was postulated that the use of these more flexible dianhydrides would result in more processable polyimides.

Influence of thermal expansion on shrinkage during photopolymerization of dental resins based on bis-GMA/TEGDMA.

PubMed

Mucci, Veronica; Arenas, Gustavo; Duchowicz, Ricardo; Cook, Wayne D; Vallo, Claudia

2009-01-01

The aim of this study was to assess volume changes that occur during photopolymerization of unfilled dental resins based on bis-GMA-TEGDMA. The resins were activated for visible light polymerization by the addition of camphorquinone (CQ) in combination with dimethylamino ethylmethacrylate (DMAEMA) or ethyl-4-dimethyl aminobenzoate (EDMAB). A fibre-optic sensing method based on a Fizeau-type interferometric scheme was employed for monitoring contraction during photopolymerization. Measurements were carried out on 10mm diameter specimens of different thicknesses (1 and 2mm). The high exothermic nature of the polymerization resulted in volume expansion during the heating, and this effect was more pronounced when the sample thickness increased. Two approaches to assess volume changes due to thermal effects are presented. Due to the difference in thermal expansion coefficients between the rubbery and glassy resins, the increase of volume due to thermal expansion was greater than the decrease in volume due to thermal contraction. As a result, the volume of the vitrified resins was greater than that calculated from polymerization contraction. The observed trends of shrinkage versus sample thickness are explained in terms of light attenuation across the path length during photopolymerization. Results obtained in this research highlight the inherent interlinking of non-isothermal photopolymerization and volumetric changes in bulk polymerizing systems.

A method for observing gas evolution during plastic laminate cure

NASA Technical Reports Server (NTRS)

Nicholls, A. H.

1969-01-01

Polyimide, phenolic, and other resins which develop volatiles during laminating or molding cure are studied using optimum cure cycles. The specimen is placed on a platen and sealed in a plastic bag, then heated and observed for gas evolution using a binocular microscope. A cover plate is added to sumulate an autoclave.

Honeycomb-laminate composite structure

NASA Technical Reports Server (NTRS)

Gilwee, W. J., Jr.; Parker, J. A. (Inventor)

1977-01-01

A honeycomb-laminate composite structure was comprised of: (1) a cellular core of a polyquinoxaline foam in a honeycomb structure, and (2) a layer of a noncombustible fibrous material impregnated with a polyimide resin laminated on the cellular core. A process for producing the honeycomb-laminate composite structure and articles containing the honeycomb-laminate composite structure is described.

Takin' the Heat

NASA Technical Reports Server (NTRS)

2001-01-01

Langley Research Center has licensed a new high-temperature polyimide with versatile applications to Unitech LLC, of Hampton, Virginia, and J. D. Lincoln, Inc., of Costa Mesa, California. Through a Memorandum of Agreement (MOA) and its license, Unitech, a client of the NASA Hampton Roads Technology Incubator (HRTI), is now selling the new polyimide, better known as RP46. Dr. Ruth Pater, of NASA Langley, developed RP46 for aerospace applications. The material was designed for re-entry vehicles and high-temperature engine components; however, its versatile nature makes it applicable as a molding, adhesive, coating, composite matrix resin, foam, or film. Available in liquid and powder forms, RP46 can also be fabricated over mesh for use in molds. RP46 presents a profitable option to manufacturers, because the ease of manufacturing the resin and the reduction in curing time saves money. Consumers save money because RP46 is more durable than similar products that are susceptible to microcracking when used as a coating or adhesive in high-temperature situations and often required reapplication. The chances of microcracking are significantly reduced with RP46 because of its unsurpased ability to resist heat and corrosion.

The effects of alumina nanofillers on mechanical properties of high-performance epoxy resin.

PubMed

Zhang, Hui; Zhang, Hui; Tang, Longcheng; Liu, Gang; Zhang, Daijun; Zhou, Lingyun; Zhang, Zhong

2010-11-01

In the past decade extensive studies have been focused on mechanical properties of inorganic nanofiller/epoxy matrices. In this work we systematically investigated the mechanical properties of nano-alumina-filled E-54/4, 4-diaminodiphenylsulphone (DDS) epoxy resins, which were prepared via combining high-speed mixing with three-roll milling. Homogeneous dispersion of nano-alumina with small agglomerates was obtained in epoxy resin, which was confirmed using transmission electron microscopy (TEM). The static/dynamic modulus, tensile strength and fracture toughness of the nanocomposites were found to be simultaneously enhanced with addition of nano-alumina fillers. About 50% and 80% increases of K(IC) and G(IC) were achieved in nanocomposite filled with 18.4 wt% alumina nanofillers, as compared to that of the unfilled epoxy resin. Furthermore, the corresponding fracture surfaces of tensile and compact tension samples were examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM) techniques in order to identify the relevant fracture mechanisms involved. Various fracture features including cavities/debonding of nanofiller, local plastic deformation as well as crack pinning/deflection were found to be operative in the presence of nano-alumina fillers.

Synthesis, kinetics and characterizations of polyimide based semi-IPN systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tai, H.J.

1992-01-01

The PMR-15 polyimide is the leading matrix resin for high performance composites for use in high temperature and thermo-oxidative environments. This resin has superior mechanical properties, good processability and a high working temperature at around 300[degrees]C. It has the disadvantages of being brittle and high susceptibility to microcracking from thermal cycling that limit its widespread application. To improve the fracture toughness, a thermoplastic polyimide, LARC-TPI, and a thermoplastic poly (amide imide), Amoco AI-10, were added individually to PMR-15 resin to form sequential semi-interpenetrating polymer networks (semi-2-IPNs). the kinetics of imidization of LARC-TPI were studied using TGA technique. Both the solventmore » and the glass transition temperature were found to greatly affect the imidization kinetics. The kinetics could be well modeled by a two-step reaction: the first step being a second order reaction followed by a first order diffusion controlled reaction as the second step. The curing of PMR-15 and PMR-15/LARC-TPI semi-IPN was investigated by DSC. A first order reaction kinetics could describe the curing process adequately, implying that the reverse Diels-Alder reaction of the Norbornene end group was the rate controlling step. The glass transition temperature played an important role. The higher the fraction LARC-TPI, the higher the glass transition temperature of the semi-IPN prepolymer, and the slower the cure reaction. From a knowledge of kinetics, the molding cycle of PMR-15 and PMR-15/LARC-TPI semi-IPNs were determined. Both PMR-15/LARC-TPI and PMR-15/AI-10 semi-IPN systems exhibited much higher fracture toughness than PMR-15, but at the compromise of a reduction in the glass transition temperature. A single glass transition temperature for each semi-IPN was observed but there was presence of special intermolecular interaction. Tg measurements and IR spectroscopy indicated that both semi-IPN systems were compatible polymer pairs.« less

Low void content autoclave molded titanium alloy and polyimide graphite composite structures.

NASA Technical Reports Server (NTRS)

Vaughan, R. W.; Jones, R. J.; Creedon, J. F.

1972-01-01

This paper discusses a resin developed for use in autoclave molding of polyimide graphite composite stiffened, titanium alloy structures. Both primary and secondary bonded structures were evaluated that were produced by autoclave processing. Details of composite processing, adhesive formulary, and bonding processes are provided in this paper, together with mechanical property data for structures. These data include -65 F, room temperature, and 600 F shear strengths; strength retention after aging; and stress rupture properties at 600 F under various stress levels for up to 1000 hours duration. Typically, shear strengths in excess of 16 ksi at room temperature with over 60% strength retention at 600 F were obtained with titanium alloy substrates.

PMR polyimide compositions for improved performance at 371 deg C

NASA Technical Reports Server (NTRS)

Vannucci, Raymond D.

1987-01-01

Studies were conducted to identify matrix resins which have potential for use at 371 C (700 F). Utilizing PMR methodology, neat resin moldings were prepared with various monomer reactants and screened for thermo-oxidative stability at 371 C (700 F) under both ambient and a four-atmosphere air pressure. The results of the resin screening studies indicate that high molecular weight (HMW) formulated resins of first (PMR-15) and second (PMR-II) generation PMR materials exhibit lower levels of weight loss at 371 C (700 F) than PMR-15 and PMR-II resins. The resin systems which exhibited the best overall balance of processability, Tg and thermo-oxidative stability at 371 C were used to prepare unidirectional Celion 6000 and T-40R graphite fiber laminates. Laminates were evaluated for thermo-oxidative stability and 371 C mechanical properties. Results of the laminate evaluation studies indicate that two of the resin compositions have potential for use in 371 C applications. The most promising resin composition provided laminates which exhibited no drop in 371 C mechanical properties and only 11 percent weight loss after 200 hr exposure to 4 atmospheres of air at 371 C.

Dental fiber-post resin base material: a review

PubMed Central

Xu, Chun; Zhang, Fu-qiang

2014-01-01

Teeth that have short clinical crown, which are not alone enough to support the definitive restoration can be best treated using the post and core system. The advantages of fiber post over conventional metallic post materials have led to its wide acceptance. In addition to that the combination of aesthetic and mechanical benefits of fiber post has provided it with a rise in the field of dentistry. Also the results obtained from some clinical trials have encouraged the clinicians to use the fiber posts confidently. Fiber posts are manufactured from pre-stretched fibers impregnated within a resin matrix. The fibers could that be of carbon, glass/silica, and quartz, whereas Epoxy and bis-GMA are the most widely used resin bases. But recently studies are also found to be going on for polyimide as possible material for the fiber post resin base as a substitute for the conventional materials. PMID:24605208

The Effect on the Flexural Strength, Flexural Modulus and Compressive Strength of Fibre Reinforced Acrylic with That of Plain Unfilled Acrylic Resin – An in Vitro Study

PubMed Central

Thomas, Tony C; K, Aswini Kumar; Krishnan, Vinod; Mathew, Anil; V, Manju

2015-01-01

Aim: The aim of this in vitro study was to compare the flexural strength, the flexural modulus and compressive strength of the acrylic polymer reinforced with glass, carbon, polyethylene and Kevlar fibres with that of plain unfilled resin. Materials and Methods: A total of 50 specimens were prepared and divided into 10 specimens each under 5 groups namely group 1- control group without any fibres, group 2 – carbon fibres, group 3- glass fibres, group 4 – polyethylene, group 5- Kevlar. Universal testing machine (Tinius olsen, USA) was used for the testing of these specimens. Out of each group, 5 specimens were randomly selected and testing was done for flexural strength using a three point deflection test and three point bending test for compressive strength and the modulus was plotted using a graphical method. Statistical analysis was done using statistical software. Results: The respective mean values for samples in regard to their flexural strength for PMMA plain, PMMA+ glass fibre, PMMA+ carbon, PMMA+ polyethylene and PMMA+ Kevlar were 90.64, 100.79, 102.58, 94.13 and 96.43 respectively. Scheffes post hoc test clearly indicated that only mean flexural strength values of PMMA + Carbon, has the highest mean value. One-way ANOVA revealed a non-significant difference among the groups in regard to their compressive strength. Conclusion: The study concludes that carbon fibre reinforced samples has the greatest flexural strength and greatest flexural modulus, however the compressive strength remains unchanged. PMID:25954696

Development of Nonelectronic Part Cyclic Failure Rates

DTIC Science & Technology

1977-12-01

Schilling, W. A., "The User-Oriented Connector," Microwave Journal, Octcber 1976 40. Schneider, C., "Military Relay Reliability," Bell Telephone...polyimide B Diallyl phthalate, melamine , -55 to 200 fluorosilicone, silicone rubber, polysulfone, epoxy resin C Polytetrafluoroethylene (teflon) -55 to 125...propagation, solid state sciences, microwave physics and electronic reliability, maintainabilitg andcompatibility. .,% -UT104, , 8. g z

The Wettability of LaRC Colorless Polyimide Resins on Casting Surfaces

NASA Technical Reports Server (NTRS)

Miner, Gilda A.; Stoakley, Diane M.; St.Clair, Anne K.; Gierow, Paul A.; Bates, Kevin

1997-01-01

Two colorless polyimides developed at NASA Langley Research Center, LaRC -CP1 and LaRC -CP2, are noted for being optically transparent, resistant to radiation, and soluble in the imide form. These materials may be used to make transparent, thin polymer films for building large space reflector/collector inflatable antennas, solar arrays, radiometers, etc. Structures such as these require large area, seamless films produced via spin casting or spray coating the soluble imide on a variety of substrates. The ability of the soluble imide to wet and spread over the mandrel or casting substrate is needed information for processing these structures with minimum waste and reprocessing, thereby, reducing the production costs. The wettability of a liquid is reported as the contact angle of the solid/liquid system. This fairly simple measurement is complicated by the porosity and the amount of contamination of the solid substrate. This work investigates the effect of inherent viscosity, concentration of polyimide solids, and solvent type on the wettability of various curing surfaces.

Effect of Boric Acid on Volatile Products of Thermooxidative Degradation of Epoxy Polymers

NASA Astrophysics Data System (ADS)

Nazarenko, O. B.; Bukhareva, P. B.; Melnikova, T. V.; Visakh, P. M.

2016-01-01

The polymeric materials are characterized by high flammability. The use of flame retardants in order to reduce the flammability of polymers can lead to the formation of toxic gaseous products under fire conditions. In this work we studied the effect of boric acid on the volatile products of thermooxidative degradation of epoxy polymers. The comparative investigations were carried out on the samples of the unfilled epoxy resin and epoxy resin filled with a boric acid at percentage 10 wt. %. The analysis of the volatile decomposition products and thermal stability of the samples under heating in an oxidizing medium was performed using a thermal mass-spectrometric analysis. It is found that the incorporation of boric acid into the polymer matrix increases the thermal stability of epoxy composites and leads to a reduction in the 2-2.7 times of toxic gaseous products

Addition polymers from 1,4,5,8-tetrahydro-1,4;5,8-diepoxyanthracene and Bis-dienes: Processable resins for high temperature application

NASA Technical Reports Server (NTRS)

Meador, Mary Ann B.

1987-01-01

1,4,5,8-Tetrahydro-1,4;5,8-diepoxyanthracene reacts with various anthracene endcapped polyimide oligomers to form Diels-Alder cycloaddition copolymers. The polymers are soluble in common organic solvents, and have molecular weights of approximately 21,000 to 32,000. Interestingly, these resins appear to be more stable in air then in nitrogen. This is shown to be due to a unique dehydration (loss of water ranges from 2 to 5 percent) at temperatures of 390 to 400 C to give thermo-oxidatively stable pentiptycene units along the polymer backbone. Because of their high softening points and good thermo-oxidative stability, the polymers have potential as processible, matrix resins for high temperature composite applications.

A simulated RTM process for fabricating polyimide (AMB-21) carbon fiber composites

NASA Technical Reports Server (NTRS)

Avva, V. Sarma; Sadler, Robert L.; Thomas, Shanon

1995-01-01

An experimental polyimide matrix, AMB-21 - supplied by NASA/LeRC, was especially formulated to be non-carcinogenic. It was also expected to be amenable to a Resin Transfer Molding Process (RTM). AMB-21 is a solid at room temperature and must be heated to a very high temperature to obtain a fluid state. However, even after heating it to a realistic high temperature, it was found to be too viscous for use in a RTM process. As a result, a promising approach was experimented leading to the introduction of the resin into a solvent solution in order to obtain a viscosity suitable for RTM. A mixture of methanol and tetrahydroferone was found to be a suitable solvent mixture. The matrix solution was introduced into carbon-fiber preform using two techniques: (1) injection of matrix into a Resin Transfer Mold after positioning the preform into the 'mold cavity', and (2) infiltration of matrix into the preform using the 'autoclave through-the-thickness transfer process'. After completing the resin transfer (infiltration) process, the 'filled' preform was heated to 300 F for one hour to reduce the solvent content. The temperature was then increased to 400 F under a vacuum to complete the solvent evaporation and to remove volatile products of the polyimide imidization. The impregnated preform was removed from the mold and press-cured at 200 psi and 600 FF for two hours. The resulting panel was found to be of reasonably good quality. This observation was based on the results obtained from short beam shear strength (700-8000 psi) tests and microscopic examination of the cross-section indicating a very low level of porosity. Further, the flash around the molded panels from the compression molding was free of porosity indicating the removal of volatiles, solvents, and other imidization products. Based on these studies, a new RTM mold containing a diaphragm capable of applying 200 psi at 600 F has been designed and constructed with the expectation that it will allow the incorporation of all of the above processing steps, including the consolidation with the preform in the mold cavity. Moreover, the new diaphragm design will enable to process larger preform panels. Processing studies with the diaphragm mold are being initiated.

Lower temperature curing thermoset polyimides utilizing a substituted norbornene endcap

NASA Technical Reports Server (NTRS)

Waters, John F.; Sukenik, Chaim N.; Kennedy, Vance O.; Livneh, Mordechai; Youngs, Wiley J.; Sutter, James K.; Meador, Mary A. B.; Burke, Luke A.; Ahn, Myong K.

1992-01-01

Methoxycarbonyl bridgehead substituted nadic diacid monomethyl ester, when used as an endcapping monomer, lowered the cure temperature of thermoset PMR polyimides without seriously affecting other desirable properties, such as glass transition temperature and thermal oxidative stability. The C-13 CP/MAS NMR of model compounds was used to follow the cure of resin systems using both the unmodified nadic endcap and the methoxycarbonyl-substituted endcap. Rheological analysis and differential scanning calorimetry DSC also provided evidence for the lower curing nature of the substituted endcap. Two regioisomers of the bridgehead-substituted endcap were isolated, and their chemical structures were elucidated by X-ray crystallography. The model compound and molecular modeling studies conducted ruled out the possibility of regioisomeric imide formation in the substituted endcaps.

Graphite fluoride as a solid lubricant in a polyimide binder

NASA Technical Reports Server (NTRS)

Fusaro, R. L.; Sliney, H. E.

1972-01-01

Polyimide resin (PI) was shown to be a suitable binder material for the solid lubricant graphite fluoride, (CF(1.1))n. Comparisons were made to similar tests using PI-bonded MOS2 films, graphite fluoride rubbed films, and MOS2 rubbed films. The results showed that, at any one specific temperature between 25 and 400 C, the wear life of PI-bonded graphite fluoride films exceeded those of the other three films by at least a factor of 2 and by as much as a factor of 60. Minimum friction coefficients for the PI-bonded films were 0.08 for graphite fluoride and 0.04 for MOS2. The rider wear rates for the two PI-bonded films at 25 C were nearly equal.

A novel addition polyimide adhesive

NASA Technical Reports Server (NTRS)

St.clair, T. L.; Progar, D. J.

1981-01-01

An addition polyimide adhesive, LARC 13, was developed which shows promise for bonding both titanium and composites for applications which require service temperatures in excess of 533 K. The LARC 13 is based on an oligomeric bis nadimide containing a meta linked aromatic diamine. The adhesive melts prior to polymerization due to its oligomeric nature, thereby allowing it to be processed at 344 kPa or less. Therefore, LARC 13 is ideal for the bonding of honeycomb sandwich structures. After melting, the resin thermosets during the cure of the nadic endcaps to a highly crosslinked system. Few volatiles are evolved, thus allowing large enclosed structures to be bonded. Preparation of the adhesive as well as bonding, aging, and testing of lap shear and honeycomb samples are discussed.

High Temperature Thermosetting Polyimide Nanocomposites Prepared with Reduced Charge Organoclay

NASA Technical Reports Server (NTRS)

Campbell, Sandi; Liang, Margaret I.

2005-01-01

The naturally occurring sodium and calcium cations found in bentonite clay galleries were exchanged with lithium cations. Following the cation exchange, a series of reduced charge clays were prepared by heat treatment of the lithium bentonite at 130 C, 150 C, or 170 C. Inductively coupled plasma (ICP) analysis showed that heating the lithium clay at elevated temperatures reduced its cation exchange capacity. Ion exchange of heat-treated clays with either a protonated alkyl amine or a protonated aromatic diamine resulted in decreasing amounts of the organic modifier incorporated into the lithium clay. The level of silicate dispersion in a thermosetting polyimide matrix was dependent upon the temperature of Li-clay heat treatment as well as the organic modification. In general, clays treated at 150 C or 170 C, and exchanged with protonated octadcylamine or protonated 2,2'-dimethlybenzidine (DMBZ) showed a higher degree of dispersion than clays treated at 130 C, or exchanged with protonated dodecylamine. Dynamic mechanical analysis showed little change in the storage modulus or T(sub g) of the nanocomposites compared to the base resin. However, long term isothermal aging of the samples showed a significant decrease in the resin oxidative weight loss. Nanocomposite samples aged in air for 1000 hours at 288 C showed of to a decrease in weight loss compared to that of the base resin. This again was dependent on the temperature at which the Li-clay was heated and the choice of organic modification.

Quality control developments for graphite/PMR15 polyimide composites materials

NASA Technical Reports Server (NTRS)

Sheppard, C. H.; Hoggatt, J. T.

1979-01-01

The problem of lot-to-lot and within-lot variability of graphite/PMR-15 prepreg was investigated. The PMR-15 chemical characterization data were evaluated along with the processing conditions controlling the manufacture of PMR-15 resin and monomers. Manufacturing procedures were selected to yield a consistently reproducible graphite prepreg that could be processed into acceptable structural elements.

The effect of water storage, elapsed time and contaminants on the bond strength and interfacial polymerization of a nanohybrid composite.

PubMed

Perriard, Jean; Lorente, Maria Cattani; Scherrer, Susanne; Belser, Urs C; Wiskott, H W Anselm

2009-12-01

To systematically characterize the effect of time lapse, water storage, and selected contaminants on the bond strength of a nanofilled dental composite. Half-dumbbell-shaped samples were fabricated out of light-polymerizing composite resin. To function as substrates they were aged for 30 days in water. Prior to bonding, the substrates' surfaces were subjected to the following treatments: 1) Removing a 0.2- to 0.4-mm layer using a fluted carbide bur; 2) grit blasting with 50 microm alumina particles; 3) etching with phosphoric acid gel; 4) grit blasting followed by etching; 5) blasting with tribochemical particles followed by silane application; 6) sanding with 400-grit paper, air aging of the adherent half-sample before bonding; 7) surface contamination with saliva; 8) surface contamination with blood. In each group (n = 30), freshly polymerized (except in group 6) adherent half-samples were bonded to the substrate half-samples by a layer of unfilled adhesive resin. Fifteen full dumbbell-shaped specimens were subjected to tensile testing after 1 h and 15 after 7 days water storage. In a positive control group, freshly cured half-samples were bonded shortly after fabrication. The tensile strength was analyzed using Weibull statistics and presented in terms of the material's characteristic strength and shape parameter. Fractographs of the two weakest and strongest samples of each group were produced. The surfaces were searched to locate hackle, wake hackle and the origin of the fracture. Surface roughness and time lapse increased the bond strength of the repaired specimens. All groups in which surface roughness was produced before bonding increased in repair strength. Post-bonding aging improved strength. Fractographs yielded interpretable data whenever larger surfaces of single phase bonding resin were present. 1) Roughening and etching an aged composite's surface prior to applying a coat of unfilled resin and the filled material increases repair bond strength by up to 100%. 2) The repair bond strength of a roughened aged composite is 25% to 30% inferior to the tensile strength of solid specimens. 3) After 7 days' storage in water, no detrimental effect could be seen from saliva or blood contamination if the surfaces were properly rinsed.

Development of autoclavable polyimides. [fabrication procedures of high temperature resistant/fiber composite

NASA Technical Reports Server (NTRS)

Orell, M. K.; Sheppard, C. H.; Vaughan, R. W.; Jones, R. J.

1974-01-01

A poly(Diels-Alder) (PDA) resin approach was investigated as a means to achieve autoclavability of high temperature resistant resin/fiber composites under mild fabrication procedures. Low void content Type A-S graphite reinforced composites were autoclave fabricated from a PDA resin/fiber prepared from an acetone:methanol:dioxane varnish. Autoclave conditions were 477K (400F) and 0.7 MN/sq m (100 psi) for up to two hours duration. After postcure at temperatures up to 589K (600F), the composites demonstrated high initial mechanical properties at temperatures up to 561K (550F). The results from isothermal aging studies in air for 1000 hours indicated potential for long-term ( 1000 hours) use at 533K (500F) and shorter-term (up to 1000 hours) at 561K (550F).

Multifunctional Composites for Improved Polyimide Thermal Stability

NASA Technical Reports Server (NTRS)

Miller, Sandi G.

2007-01-01

The layered morphology of silicate clay provides an effective barrier to oxidative degradation of the matrix resin. However, as resin thermal stability continues to reach higher limits, development of an organic modification with comparable temperature capabilities becomes a challenge. Typically, phyllosilicates used in polymer nanocomposites are modified with an alkyl ammonium ion. Such organic modifiers are not suited for incorporation into high temperature polymers as they commonly degrade below 200oC. Therefore, the development of nanoparticle specifically suited for high temperature applications is necessary. Several nanoparticles were investigated in this study, including pre-exfoliated synthetic clay, an organically modified clay, and carbon nanofiber. Dispersion of the layered silicate increases the onset temperature of matrix degradation as well as slows oxidative degradation. The thermally stable carbon nanofibers are also observed to significantly increase the resin thermal stability.

Cure Cycle Design Methodology for Fabricating Reactive Resin Matrix Fiber Reinforced Composites: A Protocol for Producing Void-free Quality Laminates

NASA Technical Reports Server (NTRS)

Hou, Tan-Hung

2014-01-01

For the fabrication of resin matrix fiber reinforced composite laminates, a workable cure cycle (i.e., temperature and pressure profiles as a function of processing time) is needed and is critical for achieving void-free laminate consolidation. Design of such a cure cycle is not trivial, especially when dealing with reactive matrix resins. An empirical "trial and error" approach has been used as common practice in the composite industry. Such an approach is not only costly, but also ineffective at establishing the optimal processing conditions for a specific resin/fiber composite system. In this report, a rational "processing science" based approach is established, and a universal cure cycle design protocol is proposed. Following this protocol, a workable and optimal cure cycle can be readily and rationally designed for most reactive resin systems in a cost effective way. This design protocol has been validated through experimental studies of several reactive polyimide composites for a wide spectrum of usage that has been documented in the previous publications.

Nano-Particle Enhanced Polymer Materials for Space Flight Applications

NASA Technical Reports Server (NTRS)

Criss, Jim M., Jr.; Powell, William D.; Connell, John W.; Stallworth-Bordain, Yemaya; Brown, Tracy R.; Mintz, Eric A.; Schlea, Michelle R.; Shofne, Meisha L.

2009-01-01

Recent advances in materials technology both in polymer chemistry and nano-materials warrant development of enhanced structures for space flight applications. This work aims to develop spacecraft structures based on polymer matrix composites (PMCs) that utilize these advancements.. Multi-wall carbon nano-tubes (MWCNTs) are expected ·to increase mechanical performance, lower coefficient of thermal expansion (CTE), increase electrical conductivity (mitigate electrostatic charge), increase thermal conductivity, and reduce moisture absorption of the resultant space structures. In this work, blends of MWCNTs with PETI-330 were prepared and characterized. The nano-reinforced resins were then resin transfer molded (RTM) into composite panels using M55J carbon fabric and compared to baseline panels fabricated from a cyanate ester (RS-3) or a polyimide (PETI-330) resin containing no MWCNTs. In addition, methods of pre-loading the fabric with the MWCNTs were also investigated. The effects of the MWCNTs on the resin processing properties and on the composite end-use properties were also determined.

Development of fire-resistant, low smoke generating, thermally stable end items for aircraft and spacecraft

NASA Technical Reports Server (NTRS)

Gagliani, J.

1978-01-01

A new approach to the problem of flammability by the use of materials obtained from foamy polyimide resins is developed. The ability of these materials to provide fire protection is demonstrated. The development of processes for producing resilient cell foam for use in aircraft seating, thermal acoustical insulation, floor and wall panels, coated glass fabrics, and molded hardware.

Synthesis of Hydrophobic, Crosslinkable Resins.

DTIC Science & Technology

1984-12-01

insoluble products, in reactions analogous to the preparation of polyimides from polyamic acids . Examples fron7 the recent literature are provided by the...Vilsmeyer formylation,using a secondary amine with formic acid and phosphorous oxychloride [471. d. Probably the most convenient method utilises...such as styrene react with Lewis acids and so the scope for Friedel Crafts reactions is limited. Stilbene and its derivatives may be employed in such

Evaluation of high temperature structural adhesives for extended service

NASA Technical Reports Server (NTRS)

Hendricks, C. L.; Hill, S. G.

1984-01-01

High temperature stable adhesive systems were evaluated for potential Supersonic Cruise Research (SCR) vehicle applications. The program was divided into two major phases: Phase I 'Adhesive Screening' evaluated eleven selected polyimide (PI) and polyphenylquinoxaline (PPQ) adhesive resins using eight different titanium (6Al-4V) adherend surface preparations; Phase II 'Adhesive Optimization and Characterization' extensively evaluated two adhesive systems, selected from Phase I studies, for chemical characterization and environmental durability. The adhesive systems which exhibited superior thermal and environmental bond properties were LARC-TPI polyimide and polyphenylquinoxaline both developed at NASA Langley. The latter adhesive system did develop bond failures at extended thermal aging due primarily to incompatibility between the surface preparation and the polymer. However, this study did demonstrate that suitable adhesive systems are available for extended supersonic cruise vehicle design applications.

En masse pyrolysis of flexible printed circuit board wastes quantitatively yielding environmental resources.

PubMed

Kim, Jang Won; Lee, Albert S; Yu, Seunggun; Han, Jeong Whan

2018-01-15

This paper reports the recycling of flexible printed circuit board (FPCB) waste through carbonization of polyimide by dual pyrolysis processes. The organic matter was recovered as pyrolyzed oil at low temperatures, while valuable metals and polyimide-derived carbon were effectively recovered through secondary high temperature pyrolysis. The major component of organics extracted from FPCB waste comprised of epoxy resins were identified as pyrolysis oils containing bisphenol-A. The valuable metals (Cu, Ni, Ag, Sn, Au, Pd) in waste FPCB were recovered as granular shape and quantitatively analyzed via ICP-OES. In attempt to produce carbonaceous material with increased degree of graphitization at low heat-treatment conditions, the catalytic effect of transition metals within FPCB waste was investigated for the efficient carbonization of polyimide films. The morphology of the carbon powder was observed by scanning electron microscopy and graphitic carbonization was investigated with X-ray analysis. The protocols outlined in this study may allow for propitious opportunities to salvage both organic and inorganic materials from FPCB waste products for a sustainable future. Copyright © 2017 Elsevier B.V. All rights reserved.

Filled and Unfilled Temperature-Dependent Epoxy Resin Blends for Lossy Transducer Substrates

PubMed Central

Eames, Matthew D.C.; Hossack, John A.

2016-01-01

In the context of our ongoing investigation of low-cost 2-dimensional (2-D) arrays, we studied the temperature-dependent acoustic properties of epoxy blends that could serve as an acoustically lossy backing material in compact 2-D array-based devices. This material should be capable of being machined during array manufacture, while also providing adequate signal attenuation to mitigate backing block reverberation artifacts. The acoustic impedance and attenuation of 5 unfilled epoxy blends and 2 filled epoxy blends—tungsten and fiberglass fillers—were analyzed across a 35°C temperature range in 5°C increments. Unfilled epoxy materials possessed an approximately linear variation of impedance and sigmoidal variation of attenuation properties over the range of temperatures of interest. An intermediate epoxy blend was fitted to a quadratic trend line with R2 values of 0.94 and 0.99 for attenuation and impedance, respectively. It was observed that a fiberglass filler induces a strong quadratic trend in the impedance data with temperature, which results in increased error in the characterization of attenuation and impedance. The tungsten-filled epoxy was not susceptible to such problems because a different method of fabrication was required. At body temperature, the tungsten-filled epoxy could provide a 44 dB attenuation of the round-trip backing block echo in our application, in which the center frequency is 5 MHz and the backing material is 1.1 mm thick. This is an 11 dB increase in attenuation compared with the fiberglass-filled epoxy in the context of our application. This work provides motivation for exploring the use of custom-made tungsten-filled epoxy materials as a substitute PCB-based substrate to provide electrical signal interconnect. PMID:19406716

New method for shielding electron beams used for head and neck cancer treatment.

PubMed

Farahani, M; Eichmiller, F C; McLaughlin, W L

1993-01-01

Shields and stents of metals with high atomic number, which are custom cast in molds from the melt, are the materials most widely used to protect surrounding tissues during treatment of skin or oral lesions with therapeutic electron beams. An improved fabrication method is to mix a polysiloxane-metal composite, which is readily cast at room temperature by combining a metal-powder/polysiloxane resin mixture with a hardening catalyst. The purpose of the present study is to compare the shielding effectiveness of two different metal-polysiloxane composites with that of conventional cast Lipowitz metal (50.1% Bi, 26.6% Pb, 13.3% Sn, 10% Cd). Also, a 2(3) factorial experiment was run to investigate the effects and interactions of metal particle size (20-microns vs 100-microns diameter), the atomic weight of the metal (304 stainless steel vs 70% Ag, 30% Cu alloy), and the presence or absence of a layer of unfilled polymer added to the forward-scatter side of the shield. The composites of different thicknesses were made by blending 90% (w/w) metal powder separately with 10% polysiloxane base and catalyst. A thin GafChromic dosimeter film was placed between the shielding material and a polystyrene base to measure the radiation shielding effect of composite disc samples irradiated with a 6-MeV electron beam normal to the flat surface of the disc. The results show that composite shields with the metal of higher atomic weight and density (Ag-Cu) combined with an additional unfilled layer are more effective than the stainless-steel composite with a similar additional unfilled layer, in terms of diminishing the dose at the surface of the polystyrene backing material.(ABSTRACT TRUNCATED AT 250 WORDS)

Thermoplastic composites for veneering posterior teeth-a feasibility study.

PubMed

Gegauff, Anthony G; Garcia, Jose L; Koelling, Kurt W; Seghi, Robert R

2002-09-01

This pilot study was conducted to explore selected commercially-available thermoplastic composites that potentially had physical properties superior to currently available dental systems for restoring esthetic posterior crowns. Polyurethane, polycarbonate, and poly(ethylene/tetrafluoroethylene) (ETFE) composites and unfilled polyurethane specimens were injection molded to produce shapes adaptive to five standardized mechanical tests. The mechanical testing included abrasive wear rate, yield strength, apparent fracture toughness (strength ratio), flexural strength, and compressive strength. Compared to commercially available dental composites, abrasion wear rates were lower for all materials tested, yield strength was greater for the filled polycarbonates and filled polyurethane resins, fracture toughness testing was invalid (strength ratios were calculated for comparison of the pilot test materials), flexural strength was roughly similar except for the filled ETFE which was significantly greater, and compressive strength was lower. Commercially available thermoplastic resin composites, such as polyurethane, demonstrate the potential for development of an artificial crown material which exceeds the mechanical properties of currently available esthetic systems, if compressive strength can be improved.

Ultrasonic mixing of epoxy curing agents

NASA Technical Reports Server (NTRS)

Hodges, W. T.; St.clair, T. L.

1983-01-01

A new technique for mixing solid curing agents into liquid epoxy resins using ultrasonic energy was developed. This procedure allows standard curing agents such as 4,4 prime-diaminodiphenyl sulfone (4,4 prime-DDS) and its 3,3 prime-isomer, (3,3 prime-DDS) to be mixed without prior melting of the curing agent. It also allows curing agents such as 4,4 prime-diaminodiphenyl sulfone (4,4 prime-DDS) and its 3,3 prime-isomer, (3,3 prime-DDS) to be mixed without prior melting of the curing agent. It also allows curing agents with very high melt temperatures such as 4,4 prime-diaminobenzophenone (4,4 prime-DABP) (242 C) to be mixed without premature curing. Four aromatic diamines were ultrasonically blended into MY-720 epoxy resin. These were 4,4 prime-DDS; 3,3 prime-DDA; 4,4 prime-DABP and 3,3 prime-DABP. Unfilled moldings were cast and cured for each system and their physical and mechanical properties compared.

Synthesis and characterization of fluorinated polyaminoquinones and fluorinated polyimides

NASA Astrophysics Data System (ADS)

Vaccaro, Eleonora

Phenolic and quinonoid compounds are widely studied in biological sciences because of their ability to chelate heavy metals like iron and copper and recently have found new applications in synthetic macromolecules. Amino- p-benzoquinone polymers, poly[(2,5-hexamethylenediamino)-1,4-benzoquinone] and poly {[2,5-(2,2'-bistrifluoromethyl)-4,4' -biphenylenediamino]1,4-benzoquinone}, were synthesized and evaluated as adhesion promoters for steel/epoxy joints. An improvement in the torsional shear strength of these joints was observed when these polymers were used as adhesion promoters. The durability of the adhesive bond was also improved after boiling water treatment, relative to untreated and silane treated joints. The improvement in adhesion could be attributed to the formation of a chelate between the polyaminoquinone (PAQ) and the iron surface and a chemical reaction between the PAQ and the epoxy resin. A low molecular weight model compound, bis[2,5-(4-methylanilido)]-1,4-benzoquinone was also used to study coupling between the epoxy adhesive and the steel surface. Electron spin resonance (ESR), atomic absorption spectroscopy and infrared spectroscopy were used to document the epoxy-coupling agent reaction and the chelate formation. Polyimides have acquired importance in the last twenty years as the most promising macromolecules for high technology applications in new materials. Their good thermo-oxidative stability is well known, as well as their high glass transition temperature. Polyimides are versatile polymers, which can be utilized for a wide range of applications: i.e., as matrices for high performance advanced composite materials, as thin films in electronic applications, as structural adhesives and sealants and as membranes for gas separation. A novel anhydride, 1,1,1-trifluoromethyl-1-pentafluorophenylethylidene-2,2-diphthalic anhydride, 8FDA, was synthesized. Five diamines were used in the synthesis of polyimides, namely p-phenylene diamine, 3,4'-oxydianiline, 2,2-bis(3-aminophenyl)hexafluoropropane, 2,2'-bis(trifluoromethyl)benzidine and 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane. A variety of structures was achieved, allowing for a thorough determination of the structure/properties relationship. The presence of the pentafluorophenyl substituent in the polyimide backbone imparted more flexibility to the 8F polyimides, as demonstrated by the low glass transition temperatures. The dielectric constant of these 8F polyimides was the lowest ever reported for polyimides. It is believed that the pentafluorophenyl group may increase the free volume and hydrophobicity of the 8F polyimides. The thermo- and thermo-oxidative stability of these 8F polyimides was also studied and appeared to be adequate for high temperature applications.

Development of high temperature service polyimide based adhesives for titanium and composite bonding applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mayhew, R.T.; Kohli, D.K.

CYTEC Engineered Materials Inc. has developed several adhesives based on LaRC{trademark} PETI-5 Polyimide Resin for bonding titanium and composite substrates. These adhesives are intended for long term service at 177{degrees}C (350{degrees}F) and are processed at 350{degrees}C (660{degrees}F) in conventional autoclaves under 50 psi pressure. Titanium lap shears range from 48.3MPa (7000 psi) at room temperature to 31MPa (4500 psi) at 177{degrees}C (350{degrees}F). Excellent metal-to-metal peels and honeycomb bonding properties are reported for these products. In addition to film adhesive, primer and paste products have been described. Pilot line quantities of several hundred square feet of the film adhesive have beenmore » produced and sampled under the CYTEC designation FM{reg_sign} x5.« less

Cytotoxic evaluation of hydroxyapatite-filled and silica/hydroxyapatite-filled acrylate-based restorative composite resins: An in vitro study.

PubMed

Chadda, Harshita; Naveen, Sangeetha Vasudevaraj; Mohan, Saktiswaren; Satapathy, Bhabani K; Ray, Alok R; Kamarul, Tunku

2016-07-01

Although the physical and mechanical properties of hydroxyapatite-filled dental restorative composite resins have been examined, the biocompatibility of these materials has not been studied in detail. The purpose of this in vitro study was to analyze the toxicity of acrylate-based restorative composite resins filled with hydroxyapatite and a silica/hydroxyapatite combination. Five different restorative materials based on bisphenol A-glycidyl methacrylate (bis-GMA) and tri-ethylene glycol dimethacrylate (TEGDMA) were developed: unfilled (H0), hydroxyapatite-filled (H30, H50), and silica/hydroxyapatite-filled (SH30, SH50) composite resins. These were tested for in vitro cytotoxicity by using human bone marrow mesenchymal stromal cells. Surface morphology, elemental composition, and functional groups were determined by scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDX), and Fourier-transformed infrared spectroscopy (FTIR). The spectra normalization, baseline corrections, and peak integration were carried out by OPUS v4.0 software. Both in vitro cytotoxicity results and SEM analysis indicated that the composite resins developed were nontoxic and supported cell adherence. Elemental analysis with EDX revealed the presence of carbon, oxygen, calcium, silicon, and gold, while the presence of methacrylate, hydroxyl, and methylene functional groups was confirmed through FTIR analysis. The characterization and compatibility studies showed that these hydroxyapatite-filled and silica/hydroxyapatite-filled bis-GMA/TEGDMA-based restorative composite resins are nontoxic to human bone marrow mesenchymal stromal cells and show a favorable biologic response, making them potential biomaterials. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

LaRC(TM)-IA Copolyimides

NASA Technical Reports Server (NTRS)

St. Clair, Terry L.; Chang, Alice C.

1995-01-01

Copolyimides modified versions of LaRC(TM)-IA thermoplastic polyimide formulated by incorporating moieties of 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA) and, alternatively, isophthaloyldiphthalic anhydride (IDPA) into LaRC(TM)-IA polymer backbones. Exhibit higher glass-transition temperatures and retain greater fractions of lower-temperature shear moduli at higher temperatures. Copolyimides spun into fibers or used as adhesives, molding powders, or matrix resins in many applications, especially in fabrication of strong, lightweight structural components of aircraft.

Fire-retardant foams

NASA Technical Reports Server (NTRS)

Gagliani, J.

1978-01-01

Family of polyimide resins are being developed as foams with exceptional fire-retardant properties. Foams are potentially useful for seat cushions in aircraft and ground vehicles and for applications such as home furnishings and building-construction materials. Basic formulations can be modified with reinforcing fibers or fillers to produce celular materials for variety of applications. By selecting reactants, polymer structure can be modified to give foams with properties ranging from high resiliency and flexibility to brittleness and rigidity.

Interfacial fracture toughness of different resin cements bonded to a lithium disilicate glass ceramic.

PubMed

Hooshmand, Tabassom; Rostami, Golriz; Behroozibakhsh, Marjan; Fatemi, Mostafa; Keshvad, Alireza; van Noort, Richard

2012-02-01

To evaluate the effect of HF acid etching and silane treatment on the interfacial fracture toughness of a self-adhesive and two conventional resin-based cements bonded to a lithium disilicate glass ceramic. Lithium disilicate glass ceramic discs were prepared with two different surface preparations consisting of gritblasted with aluminium oxide, and gritblasted and etched with hydrofluoric acid. Ceramic surfaces with a chevron shaped circular hole were treated by an optimized silane treatment followed by an unfilled resin and then three different resin cements (Variolink II, Panavia F2, and Multilink Sprint). Specimens were kept in distilled water at 37°C for 24h and then subjected to thermocycling. The interfacial fracture toughness was measured and mode of failures was also examined. Data were analysed using analysis of variance followed by T-test analysis. No statistically significant difference in the mean fracture toughness values between the gritblasted and gritblasted and etched surfaces for Variolink II resin cement was found (P>0.05). For the gritblasted ceramic surfaces, no significant difference in the mean fracture toughness values between Panavia F2 and Variolink II was observed (P>0.05). For the gritblasted and etched ceramic surfaces, a significantly higher fracture toughness for Panavia F2 than the other cements was found (P<0.05). The interfacial fracture toughness for the lithium disilicate glass ceramic system was affected by the surface treatment and the type of luting agent. Dual-cured resin cements demonstrated a better bonding efficacy to the lithium disilicate glass ceramic compared to the self-adhesive resin cement. The lithium disilicate glass ceramic surfaces should be gritblasted and etched to get the best bond when used with Panavia F2 and Multilink Sprint resin cements, whereas for the Variolink II only gritblasting is required. The best bond overall is achieved with Panavia F2. Copyright © 2011 Elsevier Ltd. All rights reserved.

Advanced Composites: Mechanical Properties and Hardware Programs for Selected Resin Matrix Materials. [considering space shuttle applications

NASA Technical Reports Server (NTRS)

Welhart, E. K.

1976-01-01

This design note presents typical mechanical properties tabulated from industrial and governmental agencies' test programs. All data are correlated to specific products and all of the best known products are presented. The data include six epoxies, eight polyimides and one polyquinoxaline matrix material. Bron and graphite are the fiber reinforcements. Included are forty-two summaries of advanced (resin matrix) composite programs in existence in the United States. It is concluded that the selection of appropriate matrices, the geometric manner in which the fibers are incorporated in the matrix and the durability of the bond between fiber and matrix establish the end properties of the composite material and the performance of the fabricated structure.

Chemical characterization of selected LDEF polymeric materials

NASA Technical Reports Server (NTRS)

Young, Philip R.; Slemp, Wayne S.

1991-01-01

Chemical characterization of selected polymeric materials which received exposure on the Long Duration Exposure Facility (LDEF) is reported. The specimens examined include silvered fluorinated ethylene propylene Teflon thermal blanket material, polysulfone, epoxy, polyimide matrix resin/graphite fiber reinforced composites, and several high performance polymer films. These specimens came from numerous LDEF locations, and thus received different environmental exposures. The results to date show no significant change at the molecular level in the polymer that survived exposure. Scanning electron and scanning tunneling microscopes show resin loss and a texturing of some specimens which resulted in a change in optical properties. The potential effect of a silicon-containing molecular contamination on these materials is addressed. The possibility of continued post-exposure degradation of some polymeric films is also proposed.

Development of DMBZ-15 High-Glass-Transition-Temperature Polyimides as PMR-15 Replacements Given R&D 100 Award

NASA Technical Reports Server (NTRS)

Chuang, Kathy

2004-01-01

PMR-15, a high-temperature polyimide developed in the mid-1970s at the NASA Lewis Research Center,1 offers the combination of low cost, easy processing, and good high-temperature performance and stability. It has been recognized as the leading polymer matrix resin for carbon-fiber-reinforced composites used in aircraft engine components. The state-of-the-art PMR-15 polyimide composite has a glass-transition temperature (Tg) of 348 C (658 F). Since composite materials must be used at temperatures well below their glass-transition temperature, the long-term use temperatures of PMR-15 composites can be no higher than 288 C (550 F). In addition, PMR-15 is made from methylene dianiline (MDA), a known liver toxin. Concerns about the safety of workers exposed to MDA during the fabrication of PMR-15 components and about the environmental impact of PMR-15 waste disposal have led to the industry-wide implementation of special handling procedures to minimize the health risks associated with this material. These procedures have increased manufacturing and maintenance costs significantly and have limited the use of PMR-15 in commercial aircraft engine components.

Solvent free low-melt viscosity imide oligomers and thermosetting polymide composites

NASA Technical Reports Server (NTRS)

Chuang, Chun-Hua (Inventor)

2012-01-01

.[.This invention relates to the composition and a solvent-free process for preparing novel imide oligomers and polymers specifically formulated with effective amounts of a dianhydride such as 2,3,3',4-biphenyltetra carboxylic dianydride (a-BPDA), at least one aromatic diamine and an endcapped of 4-phenylethynylphthalic anhydride (PEPA) or nadic anhydride to produce imide oligomers that possess a low-melt viscosity of 1-60 poise at 260-280.degree. C. When the imide oligomer melt is cured at about 371.degree. C. in a press or autoclave under 100-500 psi, the melt resulted in a thermoset polyimide having a glass transition temperature (T.sub.g) equal to and above 310.degree. C. A novel feature of this process is that the monomers; namely the dianhydrides, diamines and the endcaps, are melt processable to form imide oligomers at temperatures ranging between 232-280.degree. C. (450-535.degree. F.) without any solvent. These low-melt imide oligomers can be easily processed by resin transfer molding (RTM), vacuum-assisted resin transfer molding (VARTM) or the resin infusion process with fiber preforms e.g. carbon, glass or quartz preforms to produce polyimide matrix composites with 288-343.degree. C. (550-650.degree. F.) high temperature performance capability..]. .Iadd.This invention relates to compositions and a solvent-free reaction process for preparing imide oligomers and polymers specifically derived from effective amounts of dianhydrides such as 2,3,3',4'-biphenyltetracarboxylic dianhydride (a-BPDA), at least one aromatic polyamine and an end-cap such as 4-phenylethynyphthalic anhydride (PEPA) or nadic anhydride to produce imide oligomers that possess a low-melt viscosity of 1-60 poise at 260.degree. C.-280.degree. C..Iaddend.

Semi-2-interpenetrating polymer networks of high temperature systems

NASA Technical Reports Server (NTRS)

Hanky, A. O.; St. Clair, T. L.

1985-01-01

A semi-interpenetrating (semi-IPN) polymer system of the semi-2-IPN type is described in which a polymer of acetylene-terminated imidesulfone (ATPISO2) is cross linked in the presence of polyimidesulfone (PISO2). Six different formulations obtained by mixing of either ATPISO2-1n or ATPISO2-3n with PISO2 in three different proportions were characterized in terms of glass transition temperature, thermooxidative stability, inherent viscosity, and dynamic mechanical properties. Adhesive (lap shear) strength was tested at elevated temperatures on aged samples of adhesive scrim cloth prepared from each resin. Woven graphite (Celion 1000)/polyimide composites were tested for flexural strength, flexural modulus, and shear strength. The network polymers have properties intermediate between those of the component polymers alone, have greatly improved processability over either polyimide, and are able to form good adhesive bonds and composites, making the semi-2-IPN systems superior materials for aerospace structures.

Development and demonstration of manufacturing processes for fabricating graphite/Larc-160 polyimide structural elements, part 4, paragraph C

NASA Technical Reports Server (NTRS)

1981-01-01

Progress in the development of processes for production of Celion/LARC-160 graphite-polyimide materials, quality control methods, and the fabrication of Space Shuttle composite structure components is reported. The formulation and processing limits for three batches of resin are presented. Process improvements for simplification of the imidizing and autoclave cure cycles are described. Imidized and autoclave cured test panels were prepared. Celion/LARC-160 cure process verification and the fabrication of honeycomb sandwich panel elements and skin/stringer panels are described. C-scans of laminates imidized at 163 C to 218 C for periods from 30 to 180 minutes, and of process verification laminates made from different batches of prepreg are presented. Failure modes and load/strain characteristics of sandwich elements and C-scans of stringer to skin bond joints are also given.

Interlaminar fracture toughness of thermoplastic composites

NASA Technical Reports Server (NTRS)

Hinkley, J. A.; Johnston, N. J.; Obrien, T. K.

1988-01-01

Edge delamination tension and double cantilever beam tests were used to characterize the interlaminar fracture toughness of continuous graphite-fiber composites made from experimental thermoplastic polyimides and a model thermoplastic. Residual thermal stresses, known to be significant in materials processed at high temperatures, were included in the edge delamination calculations. In the model thermoplastic system (polycarbonate matrix), surface properties of the graphite fiber were shown to be significant. Critical strain energy release rates for two different fibers having similar nominal tensile properties differed by 30 to 60 percent. The reason for the difference is not clear. Interlaminar toughness values for the thermoplastic polyimide composites (LARC-TPI and polyimidesulfone) were 3 to 4 in-lb/sq in. Scanning electron micrographs of the EDT fracture surfaces suggest poor fiber/matrix bonding. Residual thermal stresses account for up to 32 percent of the strain energy release in composites made from these high-temperature resins.

Effect of Sizings on the Durability of High Temperature Polymer Composites

NASA Technical Reports Server (NTRS)

Allred, Ronald E.; Shin, E. Eugene; Inghram, Linda; McCorkle, Linda; Papadopoulos, Demetrios; Wheeler, Donald; Sutter, James K.

2003-01-01

To increase performance and durability of high-temperature composite for potential rocket engine components, it is necessary to optimize wetting and interfacial bonding between high modulus carbon fibers and high-temperature polyimide resins. Sizing commercially supplied on most carbon fiber are not compatible with polyimides. In this study, the chemistry of sizing on two high modulus carbon fiber (M40J and M60J, Tiray) was characterized. A continuous desizling system that uses an environmentally friendly chemical-mechanical process was developed for tow level fiber. Composites were fabricated with fibers containing the manufacturer's sizing, desized, and further treated with a reactive finish. Results of room-temperature tests after thermal aging show that the reactive finish produces a higher strength and more durable interface compared to the manufacturer's sizing. When exposed to moisture blistering tests, however, the butter bonded composite displayed a tendency to delaminate, presumably due to trapping of volatiles.

Tough, Microcracking-Resistant, High-Temperature Polymer

NASA Technical Reports Server (NTRS)

Pater, Ruth H.; Razon, Pert; Smith, Ricky; Working, Dennis; Chang, Alice; Gerber, Margaret

1990-01-01

Simultaneous synthesis from thermosetting and thermoplastic components yields polyimide with outstanding properties. Involves process in which one polymer cross-linked in immediate presence of other, undergoing simultaneous linear chain extension. New material, LaRC-RP40 synthesized from high-temperature thermosetting imide prepolymer and from thermoplastic monomer. Three significantly improved properties: toughness, resistance to microcracking, and glass-transition temperature. Shows promise as high-temperature matrix resin for variety of components of aircraft engines and for use in other aerospace structures.

Synthesis and cure mechanism characterization of phenylethynyl-terminated imide oligomers

NASA Astrophysics Data System (ADS)

Back, Susanna Branion

Polymer matrix composites (PMC) are being investigated by the Air Force for use in engine applications, which are comprised of an intermediate carbon fiber-reinforced high temperature phenylethynyl-terminated fluorinated polyimide resin. The high-temperature phenylethynyl-terminated fluorinated polyimide resin is prepared from 4-(phenylethynyl)phthalic anhydride (4-PEPA), p-phenylenediamine (p-PDA), and hexafluoroisopropylidene bisphthalic dianhydride (6FDA). In order for these materials to be exploited to their full potential, many fundamental aspects of the polymer system need to be better understood. For this study, the high-temperature cure mechanism, the chemical structures of cure reaction products, and the effect of physical properties of impurities in the 4-PEPA monomer were investigated. A phenylethynyl-terminated imide model compound, N-(3-phenoxybenzene)-4-phenylethynylphthalimide (N-PBPEP), was prepared using both industrial 4-PEPA and recrystallized 4-PEPA. The thermal cure of this low molecular weight compound was studied using a variety of analytical techniques including differential scanning calorimetry, Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance spectroscopy (NMR), and mass spectrometry (MS). N-PBPEP made from industrial 4-PEPA begins curing 25°C later than N-PBPEP made from recrystallized 4-PEPA, indicating that thermal cure is affected by the purity of the 4-PEPA starting material. Also, both versions form an 830 g/mol dimer with three possible mechanistic pathways.

Laser acoustic emission thermal technique (LAETT): a technique for generating acoustic emission in dental composites.

PubMed

Duray, S J; Lee, S Y; Menis, D L; Gilbert, J L; Lautenschlager, E P; Greener, E H

1996-01-01

This study was designed to investigate a new method for generating interfacial debonding between the resin matrix and filler particles of dental composites. A pilot study was conducted to evaluate laser-induced acoustic emission in dental resins filled with varying quantities of particles. Model systems of 50/50 BisGMA/TEGDMA resin reinforced with 0, 25, and 75 wt% 5-10 micrometers silanated BaSiO(6) were analyzed. The sample size was 3.5 mm diameter x 0.25-0.28 mm thick. A continuous wave CO2 laser (Synrad Infrared Gas Laser Model 48-1) was used to heat the composite samples. Acoustic events were detected, recorded and processed by a model 4610 Smart Acoustic Monitor (SAM) with a 1220A preamp (Physical Acoustic Corp.) as a function of laser power. Initially, the acoustic signal from the model composites produced a burst pattern characteristic of fracturing, about 3.7 watts laser power. Acoustic emission increased with laser power up to about 6 watts. At laser powers above 6 watts, the acoustic emission remained constant. The amount of acoustic emission followed the trend: unfilled resin > composite with 25 wt% BaSiO(6) > composite with 75 wt% BaSiO(6). Acoustic emission generated by laser thermal heating is dependent on the weight percent of filler particles in the composite and the amount of laser power. For this reason, laser thermal acoustic emission might be useful as a nondestructive form of analysis of dental composites.

Improved fiber retention by the use of fillers in graphite fiber/resin matrix composites

NASA Technical Reports Server (NTRS)

Gluyas, R. E.; Bowles, K. J.

1980-01-01

A variety of matrix fillers were tested for their ability to prevent loss of fiber from graphite fiber/PMR polyimide and graphite fiber/epoxy composites in a fire. The fillers tested included powders of boron, boron carbide lime glass, lead glass, and aluminum. Boron was the most effective and prevented any loss of graphite fiber during burning. Mechanical properties of composites containing boron filler were measured and compared to those of composites containing no filler.

Gas Evolution from Insulating Materials for Superconducting Coil of Iter by Gamma Ray Irradiation at Liquid Nitrogen Temperature

NASA Astrophysics Data System (ADS)

Idesaki, A.; Koizumi, N.; Sugimoto, M.; Morishita, N.; Ohshima, T.; Okuno, K.

2008-03-01

A laminated material composed of glass cloth/polyimide film/epoxy resin will be used as an insulating material for superconducting coil of International Thermonuclear Experimental Reactor (ITER). In order to keep safe and stable operation of the superconducting coil system, it is indispensable to evaluate radiation resistance of the material, because the material is exposed to severe environments such as high radiation field and low temperature of 4 K. Especially, it is important to estimate the amount of gases evolved from the insulating material by irradiation, because the gases affect on the purifying system of liquid helium in the superconducting coil system. In this work, the gas evolution from the laminated material by gamma ray irradiation at liquid nitrogen temperature (77 K) was investigated, and the difference of gas evolution behavior due to difference of composition in the epoxy resin was discussed. It was found that the main gases evolved from the laminated material by the irradiation were hydrogen, carbon monoxide and carbon dioxide, and that the amount of gases evolved from the epoxy resin containing cyanate ester was about 60% less than that from the epoxy resin containing tetraglycidyl-diaminophenylmethane (TGDDM).

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

NASA Technical Reports Server (NTRS)

Kumose, M.; Gentz, M.; Rupnowski, P.; Armentrout, D.; Kumosa, L.; Shin, E.; Sutter, J. K.

2003-01-01

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.

Space Shuttle Columbia Aging Wiring Failure Analysis

NASA Technical Reports Server (NTRS)

McDaniels, Steven J.

2005-01-01

A Space Shuttle Columbia main engine controller 14 AWG wire short circuited during the launch of STS-93. Post-flight examination divulged that the wire had electrically arced against the head of a nearby bolt. More extensive inspection revealed additional damage to the subject wire, and to other wires as well from the mid-body of Columbia. The shorted wire was to have been constructed from nickel-plated copper conductors surrounded by the polyimide insulation Kapton, top-coated with an aromatic polyimide resin. The wires were analyzed via scanning electron microscope (SEM), energy dispersive X-Ray spectroscopy (EDX), and electron spectroscopy for chemical analysis (ESCA); differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) were performed on the polyimide. Exemplar testing under laboratory conditions was performed to replicate the mechanical damage characteristics evident on the failed wires. The exemplar testing included a step test, where, as the name implies, a person stepped on a simulated wire bundle that rested upon a bolt head. Likewise, a shear test that forced a bolt head and a torque tip against a wire was performed to attempt to damage the insulation and conductor. Additionally, a vibration test was performed to determine if a wire bundle would abrade when vibrated against the head of a bolt. Also, an abrasion test was undertaken to determine if the polyimide of the wire could be damaged by rubbing against convolex helical tubing. Finally, an impact test was performed to ascertain if the use of the tubing would protect the wire from the strike of a foreign object.

DMBZ Polyimides Provide an Alternative to PMR-15 for High-Temperature Applications

NASA Technical Reports Server (NTRS)

2005-01-01

PMR-15, a high-temperature polyimide developed in the mid-1970's at the NASA Lewis Research Center, offers the combination of ease of processing, low cost, and good stability and performance at temperatures up to 288 C (500 F). This material is widely regarded as one of the leading high-temperature matrix resins for polymer-matrix-composite aircraft engine components. PMR-15 is widely used in both military and civilian aircraft engines. The current worldwide market for PMR-15 is on the order of 50,000 lb, with a total sales of around $5 to $10 million. However, PMR-15 is made from methylene dianiline (MDA), a known animal mutagen and a suspected human mutagen. Recent concerns about the safety of workers involved in the manufacture and repair of PMR-15 components have led to the implementation of costly protective measures to limit worker exposure and ensure workplace safety. In some cases, because of safety and economic concerns, airlines have eliminated PMR-15 components from engines in their fleets. Current efforts at Lewis are focused on developing suitable replacements for PMR-15 that do not contain mutagenic constituents and have processability, stability, and mechanical properties comparable to that of PMR-15. A recent development from these efforts is a new class of thermosetting polyimides based on 2,2'-dimethylbenzidine (DMBZ). Autoclave processing developed for PMR-15 composites was used to prepare low-void-content T650-35 carbon-fiber-reinforced laminates from DMBZ-15 polyimides. The glass transition temperatures of these laminates were about 50 C higher than those of the T650- 35/PMR-15 composites (400 versus 348 C). In addition, DMBZ-15 polyimide composites aged for 1000 hr in air at 288 C (500 F) had weight losses close to those of comparable PMR-15 laminates (0.9 versus 0.7 percent). The elevated (288 C) and room temperature mechanical properties of T650-35-reinforced DMBZ-15 polyimide and PMR-15 laminates were comparable. Standard Ames tests are being conducted on this diamine to assess its mutagenicity.

Development of LaRC 160/NR150B2 polyimide graphite hybrid composites. [for shuttle applications

NASA Technical Reports Server (NTRS)

Maximovich, M. G.; Bergren, O.; Lockerby, S.

1980-01-01

A method for co-curing NR150B2 and LaRC 160 prepregs into hybrid composites was developed. The processing characteristics and the properties of the hybrid composites were compared with those of laminates fabricated from the individual component prepregs. Resin forms were selected and optimized and a new NR150 formulation was investigated. The new formulation greatly facilitated the processing and the performance of this system. Quality control techniques were evaluated and developed, high quality laminates were fabricated from both individual resin systems, and hybrid laminates were successfully co-cured. Optimum hybrid forms were investigated and several novel approaches were explored. An optimum hybrid system was developed that utilizes a LaRC curing schedule but shows no degradation of mechanical properties after aging 500 hr in air at 260 C.

The effect of surface sealants with different filler content on microleakage of Class V resin composite restorations.

PubMed

Hepdeniz, Ozge Kam; Temel, Ugur Burak; Ugurlu, Muhittin; Koskan, Ozgur

2016-01-01

Microleakage is still one of the most cited reasons for failure of resin composite restorations. Alternative methods to prevent microleakage have been investigated increasingly. The aim of this study is to evaluate the microleakage in Class V resin composite restorations with or without application of surface sealants with different filler content. Ninety-six cavities were prepared on the buccal and lingual surfaces with the coronal margins located in enamel and the cervical margins located in dentin. The cavities restored with an adhesive system (Clearfil SE Bond, Kuraray, Tokyo, Japan) and resin composite (Clearfil Majesty ES-2, Kuraray, Tokyo, Japan). Teeth were stored in distilled water for 24 h and separated into four groups according to the surface sealants (Control, Fortify, Fortify Plus, and G-Coat Plus). The teeth were thermocycled (500 cycles, 5-55° C), immersed in basic fuchsine, sectioned, and analyzed for dye penetration using stereomicroscope. The data were submitted to statistical analysis by Kruskal-Wallis and Bonferroni-Dunn test. The results of the study indicated that there was minimum leakage at the enamel margins of all groups. Bonferroni-Dunn tests revealed that Fortify and GC-Coat groups showed significantly less leakage than the Control group and the Fortify Plus group at dentin margins in lingual surfaces (P < 0.05). The all surface sealants used in this study eliminated microleakage at enamel margins. Moreover, unfilled or nanofilled surface sealants were the most effective in decreasing the degree of marginal microleakage at dentin margins. However, viscosity and penetrability of the sealants could be considered for sealing ability besides composition.

Double-Vacuum-Bag Process for Making Resin-Matrix Composites

NASA Technical Reports Server (NTRS)

Bradford, Larry J.

2007-01-01

A double-vacuum-bag process has been devised as a superior alternative to a single-vacuum-bag process used heretofore in making laminated fiber-reinforced resin-matrix composite-material structural components. This process is applicable to broad classes of high-performance matrix resins including polyimides and phenolics that emit volatile compounds (solvents and volatile by-products of resin-curing chemical reactions) during processing. The superiority of the double-vacuum-bag process lies in enhanced management of the volatile compounds. Proper management of volatiles is necessary for making composite-material components of high quality: if not removed and otherwise properly managed, volatiles can accumulate in interior pockets as resins cure, thereby forming undesired voids in the finished products. The curing cycle for manufacturing a composite laminate containing a reactive resin matrix usually consists of a two-step ramp-and-hold temperature profile and an associated single-step pressure profile as shown in Figure 1. The lower-temperature ramp-and-hold step is known in the art as the B stage. During the B stage, prepregs are heated and volatiles are generated. Because pressure is not applied at this stage, volatiles are free to escape. Pressure is applied during the higher-temperature ramp-and-hold step to consolidate the laminate and impart desired physical properties to the resin matrix. The residual volatile content and fluidity of the resin at the beginning of application of consolidation pressure are determined by the temperature and time parameters of the B stage. Once the consolidation pressure is applied, residual volatiles are locked in. In order to produce a void-free, high-quality laminate, it is necessary to design the curing cycle to obtain the required residual fluidity and the required temperature at the time of application of the consolidation pressure.

A Process for Preparing 1,3-Diamino-5-Pentafluorosulfanylbenzene and Polymers Therefrom

NASA Technical Reports Server (NTRS)

St.clair, Anne K. (Inventor); St.clair, Terry L. (Inventor); Thrasher, Joseph S. (Inventor)

1991-01-01

Diamines have shown their utility in the formation of many polymers. Examples of these polymers include polyimides, polyamides, and epoxies. The properties of these polymers are often dependent on the diamine which is used to make the polymer. By the present invention, a process was developed to make a diamine containing pentafluorosulfanylbenzene moiety. This process involves two steps: the preparation of a dinitro precursor and the reduction of the dinitro compound to form the diamine. This diamine was then reacted with various dianhydrides, diacidchlorides, and epoxy resins to yield the corresponding polyimide, polyamide, and epoxy polymers. These polymers were then used to make films, a wire coating enamel, and a semi-permeable membrane. The novelty of this invention resides in the process to make the diamine. Traditionally, dinitro compounds are reduced with hydrazine or a catalyst such as palladium on charcoal. The catalyst which is used in this invention is platinum oxide. When this catalyst is used, it makes it possible to form a polymer-grade diamine.

Screening of high temperature adhesives for large area bonding

NASA Technical Reports Server (NTRS)

Stenersen, A. A.; Wykes, D. H.

1980-01-01

High temperature-resistant adhesive systems were screened for processability, mechanical and physical properties, operational capability at 589 K (600 F), and the ability to produce large area bonds of high quality in fabricating Space Shuttle components. The adhesives consisted primarily of polyimide systems, including FM34B-18, NR-150B2 (DuPont), PMR-15, LARC-13, LARC-160, Thermid 600, and AI-1130L (AMOCA). The processing studies included preparation of polyimide resins, fabrication of film adhesives, development of lay-up and cure procedures, fabrication of honeycomb sandwich panels, and fabrication of mid-plane bonded panels in joints up to 30.5 cm (12 in.) wide. The screening program included tests for tack and drape properties, reticulation and filleting characteristics, ability to produce void-free or low porosity bonds in mid-plane bonded panels, out-time stability, lap shear strength, climbing drum peel strength, and glass transition temperature (Tg). This paper describes the processing methods developed and the test results.

Design, fabrication and test of graphite/polyimide composite joints and attachments. [spacecraft control surfaces

NASA Technical Reports Server (NTRS)

Cushman, J. B.; Mccleskey, S. F.; Ward, S. H.

1982-01-01

The design, analysis, and testing performed to develop four types of graphite/polyimide (Gr/PI) bonded and bolted composite joints for lightly loaded control surfaces on advanced space transportation systems that operate at temperatures up to 561 K (550 F) are summarized. Material properties and small specimen tests were conducted to establish design data and to evaluate specific design details. Static discriminator tests were conducted on preliminary designs to verify structural adequacy. Scaled up specimens of the final joint designs, representative of production size requirements, were subjected to a series of static and fatigue tests to evaluate joint strength. Effects of environmental conditioning were determined by testing aged (125 hours at 589 K (600 F)) and thermal cycled (116 K to 589 K (-250 F to 600 F), 125 times) specimens. It is concluded Gr/PI joints can be designed and fabricated to carry the specified loads. Test results also indicate a possible resin loss or degradation of laminates after exposure to 589 K (600 F) for 125 hours.

Diverse Electron-Induced Optical Emissions from Space Observatory Materials at Low Temperatures

NASA Technical Reports Server (NTRS)

Dennison, J.R.; Jensen, Amberly Evans; Wilson, Gregory; Dekany, Justin; Bowers, Charles W.; Meloy, Robert

2013-01-01

Electron irradiation experiments have investigated the diverse electron-induced optical and electrical signatures observed in ground-based tests of various space observatory materials at low temperature. Three types of light emission were observed: (i); long-duration cathodoluminescence which persisted as long as the electron beam was on (ii) short-duration (<1 s) arcing, resulting from electrostatic discharge; and (iii) intermediate-duration (100 s) glow-termed "flares". We discuss how the electron currents and arcing-as well as light emission absolute intensity and frequency-depend on electron beam energy, power, and flux and the temperature and thickness of different bulk (polyimides, epoxy resins, and silica glasses) and composite dielectric materials (disordered SiO2 thin films, carbon- and fiberglass-epoxy composites, and macroscopically-conductive carbon-loaded polyimides). We conclude that electron-induced optical emissions resulting from interactions between observatory materials and the space environment electron flux can, in specific circumstances, make significant contributions to the stray light background that could possibly adversely affect the performance of space-based observatories.

A Limited Comparison of the Thermal Durability of Polyimide Candidate Matrix Polymers with PMR-15

NASA Technical Reports Server (NTRS)

Bowles, Kenneth J.; Papadopoulos, Demetrios S.; Scheiman, Daniel A.; Inghram, Linda L.; McCorkle, Linda S.; Klans, Ojars V.

2003-01-01

Studies were conducted with six different candidate high-temperature neat matrix resin specimens of varied geometric shapes to investigate the mechanisms involved in the thermal degradation of polyimides like PMR-15. The metrics for assessing the quality of these candidates were chosen to be glass transition temperature (T(sub g)), thermo-oxidative stability, dynamic mechanical properties, microstructural changes, and dimensional stability. The processing and mechanical properties were not investigated in the study reported herein. The dimensional changes and surface layer growth were measured and recorded. The data were in agreement with earlier published data. An initial weight increase reaction was observed to be dominating at the lower temperatures. However, at the more elevated temperatures, the weight loss reactions were prevalent and probably masked the weight gain reaction. These data confirmed the findings of the existence of an initial weight gain reaction previously reported. Surface- and core-dependent weight losses were shown to control the polymer degradation at the higher temperatures.

Survivability of Affordable High Temperature Polymer Matrix Composites for Propulsion Engine Components

NASA Technical Reports Server (NTRS)

Dean, Derrick; Haque, Anwar; Vaidya, Uday; Meador, Michael A. (Technical Monitor)

2003-01-01

PMR-type polyimides are regarded as state of the art high temperature polymers, due to their excellent thermo-mechanical properties and thermo-oxidative stability. One of their drawbacks, however is the inability to process them using cost-effective processing methods such as Resin Transfer Molding (RTM) and Resin Film Infusion (RFI). Development of low viscosity, high temperature polymers has been the subject of intense research. Recently, a new generation of low viscosity polyimides were synthesized by the introduction of twisted biphenyl or binapthyl groups into the backbone. This report details the progress for Year 1, which has involved acquiring samples and initiating Phases I and II of the proposed research. Specifically, studies of the process-property relationships of a series of polymers using oligomers based on 2,3,3' ,4'-biphenyltertracarboxylic dianhydride (PBDA) and a mixture of a diamine, BAX and a triamine, 1,3,5-Tris (4-aminophenoxybenzene), TAB, where the amount of TAB was varied have been initiated. The sample containing 10 percent TAB possesses a slightly higher degree of crystalline order versus that of the 20 percent TAB sample, based on x-ray diffraction studies of the b-staged oligomers. Both systems lose all of the crystalline order upon curing, however. The chemorheology has been studied as a function of the TAB content. While the magnitude of the viscosity is essentially the same for both systems, the cure kinetics of the 10 percent TAB system is faster than that for the 20 percent TAB system. The sample exhibits a melting-recrystallization-remelting behavior before the crosslinking commences. Correlation of other kinetic parameters, such as the activation energies for curing, the Tg and mechanical properties to the structure of these systems is underway. Future studies will involve characterization of mechanical and thermal properties of the pure resins and the fabrication of fiber reinforced composites using these materials.

Hybridized polymer matrix composites

NASA Technical Reports Server (NTRS)

House, E. E.; Hoggatt, J. T.; Symonds, W. A.

1980-01-01

The extent to which graphite fibers are released from resin matrix composites that are exposed to fire and impact conditions was determined. Laboratory simulations of those conditions that could exist in the event of an aircraft crash and burn situation were evaluated. The effectiveness of various hybridizing concepts in preventing this release of graphite fibers were also evaluated. The baseline (i.e., unhybridized) laminates examined were prepared from commercially available graphite/epoxy, graphite/polyimide, and graphite/phenolic materials. Hybridizing concepts investigated included resin fillers, laminate coatings, resin blending, and mechanical interlocking of the graphite reinforcement. The baseline and hybridized laminates' mechanical properties, before and after isothermal and humidity aging, were also compared. It was found that a small amount of graphite fiber was released from the graphite/epoxy laminates during the burn and impact conditions used in this program. However, the extent to which the fibers were released is not considered a severe enough problem to preclude the use of graphite reinforced composites in civil aircraft structure. It also was found that several hybrid concepts eliminated this fiber release. Isothermal and humidity aging did not appear to alter the fiber release tendencies.

Thermoplastic adhesives based on 4,4'-isophthaloyldiphthalic anhydride (IDPA)

NASA Technical Reports Server (NTRS)

Progar, Donald J.; Stclair, Terry L.; Pratt, J. Richard

1988-01-01

Thermoplastic polyimides were prepared and evaluated as adhesives. These materials are based on 4,4'-isophthaloyldiphathalic anhydride (IDAP) and either metaphenylene diamine (MPD) or 3,3'-diaminobenzophenone (DBAP). Both polymers exhibit excellent adhesive properties; however, the IDPA-MPD is the more attractive system because of a combination of high mechanical and physical properties as well as being made from commercially attractive monomers. The IDPA-MPD is an isomeric form of the commercially available adhesive and matrix resin, LARC-TPI and both systems have the same glass transition temperature and exhibit similar adhesive properties.

Flexible Circuits

NASA Technical Reports Server (NTRS)

1986-01-01

Adflex Solutions, Inc.'s flexible circuits may be molded to the shape of a chassis for bulk reduction. Particularly valuable when circuitry must be moved. They are produced by combining a plastic film, a metallic conductor and an adhesive. One adhesive, LARC-TPI, developed by the Langley Research Center, is a thermoplastic polyimide resin used to produce laminates by Rogers Corporation. It can be processed at a lower temperature, has good moisture resistance and excellent adherence. It is used to bond film to copper foil conductor materials in flexible circuits. The circuits have both aerospace and commercial applications.

Chemical approach for controlling nadimide cure temperature and rate

NASA Technical Reports Server (NTRS)

Lauver, R. W. (Inventor)

1985-01-01

Polyimide resins suitable for use as composite matrix materials are formed by copolymerization of maleic and norbornenyl end-capped monomers and oligomers. The copolymers can be cured at temperatures under about 300 C. by controlling the available concentration of the maleic end-capped reactant. This control can be achieved by adding sufficient amounts of said maleic reactant, or by chemical modification of either copolymer, to increase Diels-Alder retrogression of the norbornenyl-capped reactant and/or holding initiation and polymerization to a rate compatible with the availability of the maleic-capped reactant.

Chemical approach for controlling nadimide cure temperature and rate

NASA Technical Reports Server (NTRS)

Lauver, R. W. (Inventor)

1984-01-01

Polyimide resins suitable for use as composite matrix materials are formed by copolymerization of maleic and norbornenyl endcapped monomers and oligomers. The copolymers can be cured at temperatures under about 300 C by controlling the available concentration of the maleic capped reactant. This control can be achieved by adding sufficient amounts of said maleic reactant, or by chemical modification of either copolymer, so as to either increase Diels-Alder retrogression of the norbornenyl capped reactant and/or holding initiation and polymerization to a rate compatible with the availability of the maleic capped reactant.

Polymer matrix composites research at NASA Lewis Research Center

NASA Technical Reports Server (NTRS)

Serafini, T. T.

1982-01-01

The in situ polymerization of monomer reactants (PMR) approach was demonstrated to be a powerful approach for solving many of the processing difficulties associated with the use of high temperature resistant polymers as matrix resins in high performance composites. The PMR-15 polyimide provides the best overall balance of processing characteristics and elevated temperature properties. The excellent properties and commercial availability of composite materials based on PMR-15 led to their acceptance as viable engineering materials. The PMR-15 composites are used to produce a variety of high quality structural components.

Chemical approach for controlling nadimide cure temperature and rate

NASA Technical Reports Server (NTRS)

Lauver, R. W. (Inventor)

1985-01-01

Polyimide resins suitable for use as composite matrix materials are formed by copolymerization of maleic and norbornenyl endcapped monomers and oligomers. The copolymers can be cured at temperatures under about 300 C by controlling the available concentration of the maleic endcapped reactant. This control is achieved by adding sufficient amounts of said maleic reactant or by chemical modification of either copolymer, to either increase Diels-Alder retrogression of the norbornenyl capped reactant and/or hold initiation and polymerization to a rate compatible with the availability of the maleic capped reactant.

Heatshield material selection for advanced ballistic reentry vehicles. [rayon fiber cloth impregnated with phenolic resin

NASA Technical Reports Server (NTRS)

Legendre, P. J.; Holtz, T.; Sikra, J. C.

1980-01-01

The Performance of staple rayon fiber and AVTEX continuous rayon fiber was evaluated as precursor materials for heatshields. The materials studied were referenced to the IRC FM5055A heatshield materials flown during the past decade. Three different arc jet facilities were used to simulate portions of the reentry environment. The IRC FM5055A and the AVTEX FM5055G, both continuous rayon fiber woven materials having the phenolic impregnant filled with carbon particles were compared. The AVTEX continuous fiber, unfilled material FM5822A was also examined to a limited extent. Test results show that the AVTEX FM5055G material provided a close substitute for the IRC FM5055A material both in terms of thermal protection and roll torque performance.

RTM370 Polyimide Braided Composites: Characterization and Impact Testing

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.; Revilock, Duane M.; Ruggeri, Charles R.; Criss, Jim M., Jr.; Mintz, Eric A.

2013-01-01

RTM370 imide oligomer based on 2,3,3',4'-biphenyl dianhydride (a-BPDA), 3,4'-oxydianiline (3,4'-ODA) and terminated with the 4-phenylethynylphthalic (PEPA) endcap has been shown to exhibit a low melt viscosity (10-30 poise) at 280 C with a pot-life of 1-2 h and a high cured glass transition temperature (Tg) of 370 C. RTM370 resin has been successfully fabricated into composites reinforced with T650-35 carbon fabrics by resin transfer molding (RTM). RTM370 composites display excellent mechanical properties up to 327 C (620 F), and outstanding property retention after aging at 288degC (550 F) for 1000 h, and under hot-wet conditions. In ballistic impact testing, RTM370 triaxial braided T650-35 carbon fiber composites exhibited enhanced energy absorption at 288 C (550 F) compared to ambient temperature.

Approaches to New Endcaps for Improved Oxidation Resistance

NASA Technical Reports Server (NTRS)

Meador, Mary Ann B.; Frimer, Aryeh A.

1999-01-01

Norbornenyl-end capped PMR polyimide resins are widely used as polymer matrix composite materials for aircraft engine applications, since they combine ease of processing with good oxidative stability up to 300 C. PMR resins are prepared by a two-step approach involving the initial formation of oligomeric pre-polymers capped at both ends by a latent reactive end cap. The end cap undergoes cross-linking during higher temperature processing, producing the desired low density, high specific strength materials, for PMR- 15. The end cap facilitates processing by controlling the molecular weight of the oligomer and allowing flow before it cross-links. However, after cross-linking, this very end cap accounts for much of the weight loss in the polymer on aging in air at elevated temperatures. Understanding this degradation provides clues for designing new end caps to slow down degradation, and prolong the lifetime of the material.

Influence of gamma ray irradiation on thermal conductivity of bismaleimide-triazine-based insulation tape at cryogenic temperature

NASA Astrophysics Data System (ADS)

Yang, Y.; Yoshida, M.; Idesaki, A.; Ogitsu, T.

2018-01-01

Recent accelerator-based experiments for particle physics require the superconducting magnets that can be operated under high radiation environment. An electrical insulation tape, which is composed of polyimide film and a boron free glass fabric pre-impregnated with epoxy resin blended with bismaleimide-triazine resin, is developed to enhance the radiation tolerance for superconducting magnets. Since the thermal conductivity of insulation tape is one of key parameters that affects the coil temperature during the operation, the influence of gamma-ray irradiation on the thermal conductivity of the insulation tape is investigated with a maximum dose of 5 MGy. The thermal conductivity is measured at cryogenic temperature from 5 K to 20 K cooled by a Gifford-McMahon cryocooler. By comparing the thermal conductivity before and after the gamma ray irradiation, no significant degradation on the thermal conductivity has been observed.

Flexible Bionanocomposites from Epoxidized Hemp Seed Oil Thermosetting Resin Reinforced with Halloysite Nanotubes.

PubMed

Shuttleworth, Peter S; Díez-Pascual, Ana M; Marco, Carlos; Ellis, Gary

2017-03-23

Hemp seed (Cannabis sativa L.) oil comprises a variety of beneficial unsaturated triglycerides with well-documented nutritional and health benefits. However, it can become rancid over a relatively short time period, leading to increased industrial costs and waste of a valuable product. The development of sustainable polymers is presented as a strategy, where both the presence of unsaturation and peroxide content could be effectively used to alleviate both the waste and financial burden. After the reaction with peroxyacetic acid, the incorporation of halloysite nanotubes (HNTs), and the subsequent thermal curing, without the need for organic solvents or interfacial modifiers, flexible transparent materials with a low glass-transition temperature were developed. The improvement in the thermal stability and both the static and dynamic mechanical properties of the bionanocomposites were significantly enhanced with the well-dispersed HNT filler. At an optimum concentration of 0.5 wt % HNTs, a simultaneous increase in stiffness, strength, ductility, and toughness was observed in comparison to the unfilled cured resin. These sustainable food-waste-derived bionanocomposites may provide an interesting alternative to petroleum-based materials, particularly for low-load-bearing applications, such as packaging.

Effect of Glass Fiber Incorporation on Flexural Properties of Experimental Composites

PubMed Central

Fonseca, Rodrigo Borges; Marques, Aline Silva; Bernades, Karina de Oliveira; Carlo, Hugo Lemes; Naves, Lucas Zago

2014-01-01

This study evaluated the effect of fiber addiction in flexural properties of 30 wt% silica filled BisGMA resin (FR) or unfilled Bis-GMA (UR). Ten groups were created (N = 10) varying the resin (FR or UR) and quantity of glass fibers (wt%: 0, 10, 15, 20, and 30). Samples (10 × 2 × 1 mm) were submitted to flexural strength test following SEM examination. Data were analyzed by two-way ANOVA, Tukey, and Student t-test (α = 0.05). Results for flexural strength (MPa) were FR-groups: 0% (442.7 ± 140.6)C, 10% (772.8 ± 446.3)ABC, 15% (854.7 ± 297.3)AB, 20% (863.4 ± 418.0)A, 30% (459.5 ± 140.5)BC; UR-groups: 0% (187.7 ± 120.3)B, 10% (795.4 ± 688.1)B, 15% (1999.9 ± 1258.6)A, 20% (1911.5 ± 596.8)A, and 30% (2090.6 ± 656.7)A, and for flexural modulus (GPa) FR-groups: 0% (2065.63 ± 882.15)B, 10% (4479.06 ± 3019.82)AB, 15% (5694.89 ± 2790.3)A, 20% (6042.11 ± 3392.13)A, and 30% (2495.67 ± 1345.86)B; UR-groups: 0% (1090.08 ± 708.81)C, 10% (7032.13 ± 7864.53)BC, 15% (19331.57 ± 16759.12)AB, 20% (15726.03 ± 8035.09)AB, and 30% (29364.37 ± 13928.96)A. Fiber addiction in BisGMA resin increases flexural properties, and the interaction between resin and fibers seems better in the absence of inorganic fillers increasing flexural properties. PMID:25136595

Effect of glass fiber incorporation on flexural properties of experimental composites.

PubMed

Fonseca, Rodrigo Borges; Marques, Aline Silva; Bernades, Karina de Oliveira; Carlo, Hugo Lemes; Naves, Lucas Zago

2014-01-01

This study evaluated the effect of fiber addiction in flexural properties of 30 wt% silica filled BisGMA resin (FR) or unfilled Bis-GMA (UR). Ten groups were created (N = 10) varying the resin (FR or UR) and quantity of glass fibers (wt%: 0, 10, 15, 20, and 30). Samples (10 × 2 × 1 mm) were submitted to flexural strength test following SEM examination. Data were analyzed by two-way ANOVA, Tukey, and Student t-test (α = 0.05). Results for flexural strength (MPa) were FR-groups: 0% (442.7 ± 140.6)(C), 10% (772.8 ± 446.3)(ABC), 15% (854.7 ± 297.3)(AB), 20% (863.4 ± 418.0)(A), 30% (459.5 ± 140.5)(BC); UR-groups: 0% (187.7 ± 120.3)(B), 10% (795.4 ± 688.1)(B), 15% (1999.9 ± 1258.6)(A), 20% (1911.5 ± 596.8)(A), and 30% (2090.6 ± 656.7)(A), and for flexural modulus (GPa) FR-groups: 0% (2065.63 ± 882.15)(B), 10% (4479.06 ± 3019.82)(AB), 15% (5694.89 ± 2790.3)(A), 20% (6042.11 ± 3392.13)(A), and 30% (2495.67 ± 1345.86)(B); UR-groups: 0% (1090.08 ± 708.81)(C), 10% (7032.13 ± 7864.53)(BC), 15% (19331.57 ± 16759.12)(AB), 20% (15726.03 ± 8035.09)(AB), and 30% (29364.37 ± 13928.96)(A). Fiber addiction in BisGMA resin increases flexural properties, and the interaction between resin and fibers seems better in the absence of inorganic fillers increasing flexural properties.

The effect of surface sealants with different filler content on microleakage of Class V resin composite restorations

PubMed Central

Hepdeniz, Ozge Kam; Temel, Ugur Burak; Ugurlu, Muhittin; Koskan, Ozgur

2016-01-01

Objective: Microleakage is still one of the most cited reasons for failure of resin composite restorations. Alternative methods to prevent microleakage have been investigated increasingly. The aim of this study is to evaluate the microleakage in Class V resin composite restorations with or without application of surface sealants with different filler content. Materials and Methods: Ninety-six cavities were prepared on the buccal and lingual surfaces with the coronal margins located in enamel and the cervical margins located in dentin. The cavities restored with an adhesive system (Clearfil SE Bond, Kuraray, Tokyo, Japan) and resin composite (Clearfil Majesty ES-2, Kuraray, Tokyo, Japan). Teeth were stored in distilled water for 24 h and separated into four groups according to the surface sealants (Control, Fortify, Fortify Plus, and G-Coat Plus). The teeth were thermocycled (500 cycles, 5–55° C), immersed in basic fuchsine, sectioned, and analyzed for dye penetration using stereomicroscope. The data were submitted to statistical analysis by Kruskal–Wallis and Bonferroni–Dunn test. Results: The results of the study indicated that there was minimum leakage at the enamel margins of all groups. Bonferroni–Dunn tests revealed that Fortify and GC-Coat groups showed significantly less leakage than the Control group and the Fortify Plus group at dentin margins in lingual surfaces (P < 0.05). Conclusion: The all surface sealants used in this study eliminated microleakage at enamel margins. Moreover, unfilled or nanofilled surface sealants were the most effective in decreasing the degree of marginal microleakage at dentin margins. However, viscosity and penetrability of the sealants could be considered for sealing ability besides composition. PMID:27095890

Process engineering of polynanomeric layered and infused composites

NASA Astrophysics Data System (ADS)

Williams, Ebonee Porche Marie

As the application of advanced polymeric composites expands, the continued adaptation of traditional as well as the incorporation and/or implementation of new technologies continue to be at the core of development for engineers. One of these traditional technologies is honeycomb sandwich composites. This technology has been around for more than fifty years and there have been minimal alterations to the materials used to produce the parts and the process used to manufacture the structures. This is where the depth of this work focused. Traditional honeycomb core dip resin systems were modified to incorporate nano scale fillers. This adaptation is one of the defining aspects of polynanomeric systems, the concept of which is that modifications of the nano scale in a polymer system create nano layered structures that emulate the properties of both the polymer and the nano filler, a nano composite. The modified resin systems were characterized to investigate morphology, thermal and mechanical properties as well as electrical characteristics. It was observed that the nano altered resin system exhibited increased mechanical, 50 to 60%, and thermal properties, burn temperatures extended by 30°C, while also demonstrating improved electrical properties. These were significant results given that the main applications of honeycomb sandwich structures are on the interior of aircrafts. These results could open the door to some new applications of the modified resin system. This work also implemented a new processing technique to produce honeycomb sandwich structures. The technique was Vacuum Assisted Resin Transfer Molding, VARTM, which has gained interest over the last decade due to the reduced up front cost to initiate production, the ease of processing, and the overall health benefits. This process was successfully performed to produce sandwich structures by incorporating a permeable scrim layer at the core face sheet interface. This was the first successful production of unfilled honeycomb core sandwich part production. Overall this work is at the tip of implementing new materials and processing techniques into honeycomb core and honeycomb sandwich composite structures.

Fabrication and Electromagnetic Characterization of Novel Self-Metallized Thin Films

NASA Technical Reports Server (NTRS)

Mackenzie, Anne I.; Cravey, Robin L.; Dudley, Kenneth L.; Fralick, Dion T.; Miner, Gilda A.; Stoakley, Diane M.

2002-01-01

Unique, self-metallized films were investigated for deployable reflector antenna applications at L-band. Polyamic acid resins or soluble polyimides were doped with metal complexes, cast into films, and thermally cured. Each resulting film had a metallic layer on one side, adhering unfailingly to the polymer. Metallization was successful for silver or palladium in 3,3',4,4'-benzophenonetetracarboxylic acid dianhydride (BTDA) and 4,4'- oxydianiline and for gold in BTDA and 2,2-bis[4-(4- aminophenoxy)phenyl]hexafluoropropane (4-BDAF) or the space durable polyimide, 2,2-bis(3,4-dicarboxyphenyl)- hexafluoropropane dianhydride and 4-BDAF (LaRCCP1). Reflectivity, transmissivity, and emissivity were determined, using an HP 8510 Vector Network Analyzer, to within 0.001 precision and accuracy. A custom-made test fixture/positioner, a thru-reflect-line calibration, and calculated reflection coefficients were used. The Ag film proved most suitable for further study, with 0.9957 reflectivity and 0.0042 emissivity. The Pd films were 0.89 reflective and 0.11 emissive; both Au films tested entirely transmissive. Transmission and scanning electron micrographs, S-parameters, and power coefficients are shown.

Phenylethynyl Containing Polyarylene Ethers/Polyimides Resin Infiltration of Composites

NASA Technical Reports Server (NTRS)

Dunn, DeRome O.

1998-01-01

The following tasks were performed at NCA&TSU during the second year in performance of the grant. LaRC-LV-1 13 resin was synthesized at NCA&TSU. In order to perform the synthesis, glassware and needed apparatus were purchased with grant funds along with the appropriate monomers. It was found that the LaRC-LV-1 13 resin was easily synthesized by the NMP solvent/toluene imminization/distilled water precipitation process. However, in use this resin exhibited a bubbling/foaming behavior during cure that was detrimental leading to the production of composite panels having a high void content. Composite panels were fabricated using compression molding and resin transfer molding (RTM) techniques. Initial fiber volume determinations were computed at NCA&TSU along with NASA-Langley measured c-scans on the panels produced. The initial results indicated a unsatisfactory level of approximately 20% by volume of voids. Testing of uniaxial coupons in compression to failure also agreed with these results. The uniaxial coupons delaminated as the major mode of failure indicative of an unacceptably low level of resin and to much void content in the final composites produced. In discussions with Dr. Brian Jensen, it was suggested the void fraction needs to be reduced to at least 2% by volume for a useful composite. The panels produced used both resin synthesized at NASA-Langley and NCA&TSU. In reviewing our progress over the past year, it was noted that the resin as formulated by the current synthesis process bubbled at elevated temperature. This was especially observed in neat resin slugs cured at the recommended one, four and eight hour cure temperatures. Pressurized cures where then performed with pressures up to 200 psi and simultaneously the lowest eight hour cure temperatures. Although this procedure reduced the amount of bubbles to some extent in the neat resin slugs it did not completely eliminate them. The cure reaction appears to be very energetic even at the lowest recommended cure temperature. Currently, the pressurized cure apparatus developed at NCA&TSU is limited to 200 psi.

Photoluminescence and electrical characterization of unfilled tetragonal tungsten bronze Ba{sub 4}La{sub 1−x}Eu{sub x}TiNb{sub 9}O{sub 30}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wei, T., E-mail: weitong.nju@gmail.com; Wang, Y.Q.; Zhao, C.Z.

Graphical abstract: PL spectra of the unfilled TTB structure BLTN: Eu{sup 3+}x samples (x = 0.00, 0.25, 0.50, 0.75, and 1.00) excited by 399 nm. The inset is a schematic diagram of the unfilled TTB structure. - Highlights: • Unfilled TTB structure BLTN: Eu{sup 3+}x ceramics have been synthesized. • Photoluminescenct properties of the BLTN: Eu{sup 3+}x ceramics have been first reported. • Bright red emission excited by NUV light has been observed at room temperature. • Obvious variations of dielectric characteristics have been confirmed. • Relaxor-like ferroelectric phase transitions have been detected. - Abstract: Unfilled tetragonal tungsten bronze (TTB)more » structure Ba{sub 4}LaTiNb{sub 9}O{sub 30} doped by Eu{sup 3+} (BLTN: Eu{sup 3+}x) with different x have been prepared, and their structural, photoluminescence, dielectric, and ferroelectric properties are carefully investigated in this work. Bright red emission, originating from {sup 5}D{sub 0} → {sup 7}F{sub 1} and {sup 5}D{sub 0} → {sup 7}F{sub 2} transitions of Eu{sup 3+} ions, has been observed by naked eyes at room temperature under near ultraviolet (NUV) light excitation. Optimized emission intensity is obtained when x = 1.00 for present unfilled TTB-type BLTN: Eu{sup 3+}x samples. Furthermore, with increasing x, the dielectric and ferroelectric characteristics of the unfilled TTB-type BLTN: Eu{sup 3+}x samples also display remarkable variation. When x ≥ 0.50 relaxor-like ferroelectric phase transitions are detected above room temperature, it is believed that unfilled TTB-type BLTN: Eu{sup 3+}x = 1.00 involving bright photoluminescence and enhanced ferroelectric properties may act as a potentially multifunctional optical-electro material.« less

Incidence of flare-ups and evaluation of quality after retreatment of resorcinol-formaldehyde resin ("Russian Red Cement") endodontic therapy.

PubMed

Gound, Tom G; Marx, David; Schwandt, Nathan A

2003-10-01

The purpose of this retrospective study was to evaluate the quality of treatment and incidence of flare-ups when teeth with resorcinol-formaldehyde resin are retreated in a postgraduate endodontic clinic. Fifty-eight cases were included in this study. Obturated and unfilled canal space was measured on radiographs. Forty-eight percent of the total canal space was filled before retreatment; 90% was filled after retreatment. After retreatment, obturations were rated as optimal in 59%, improved in 33%, unchanged in 6%, and worse in 2%. Seven patients (12%) had postretreatment flare-ups. Data were statistically analyzed using the Cochran-Armitage Test for Discrete Variables. No statistical difference in the incidence of flare-ups was found in teeth that before treatment had more than half the canal space filled compared to teeth with less than half, cases with pre-existing periradicular radiolucencies compared to cases with normal periradicular appearance, symptomatic cases compared to asymptomatic cases, or cases with optimal fillings after retreatment compared to less than optimal cases. It was concluded that teeth with resorcinol-formaldehyde fillings might be retreated with a good prognosis for improving the radiographic quality, but a higher than normal incidence of flare-ups may occur.

Effect of substituted phenylnadimides on processing and properties of PMR polyimide composites

NASA Technical Reports Server (NTRS)

Alston, W. B.; Lauver, R. W.

1985-01-01

Three nitrophenylnadimide cure initiators and two phenylnadimides (without nitros) were evaluated as additives to PMR-15 resins and Celion 6000 graphite fiber composites. The results of a resin screening study eliminated all of the additives except 3-nitrophenylnadimide (NO2PN) for use as a low temperature curing additive for PMR-15. Thus, NO2PN and the two control additives were investigated in PMR-15 formulations from which Celion 6000 graphite fiber/PMR-15 composites were processed both with low temperature (274 C) and normal (316 C) cure cycles. Comparisons of the two processing cycles, the resultant glass transition temperatures (Tg), the ambient, 274 and 316 C composite mechanical properties determined before and after 316 C postcure, the 316 C thermo-oxidative weight losses and the retention of 316 C composite mechanical properties are presented. Empirical correlations of the type and amount of nadimide additives with processing parameters, Tg, composite mechanical properties, composite thermo-oxidative stability and long term retention of 316 C composite mechanical properties are also presented.

Effects of graphite fiber stability on the properties of PMR polyimide composites

NASA Technical Reports Server (NTRS)

Delvigs, P.; Alston, W. B.; Vannucci, R. D.

1979-01-01

The effect of the stability of graphite fibers on composite properties after exposure in air at 600 F was investigated. Composites were fabricated from PMR-15 and PMR-2 monomer solutions, using HTS-2 and Celion 6000 graphite fibers as the reinforcement. The effect of long-term exposure in air at 600 F on composite weight loss and mechanical properties was determined. These composites exhibited a significantly increased lifetime at that temperature compared to composites fabricated from HTS fiber sold prior to 1975. The effect of the PMR-15 and PMR-II resin compositions on long-term composite performance at 600 F is also discussed.

Rigid zeolite containing polyurethane foams

DOEpatents

Frost, Charles B.

1985-01-01

A closed cell rigid polyurethane foam has been prepared which contains up to about 60% by weight of molecular sieves capable of sorbing molecules with effective critical diameters of up to about 10 .ANG.. The molecular sieve component of the foam can be preloaded with catalysts or with reactive compounds that can be released upon activation of the foam to control and complete crosslinking after the foam is formed. The foam can also be loaded with water or other flame-retarding agents, after completion. Up to about 50% of the weight of the isocyanate component of the foam can be replaced by polyimide resin precursors for incorporation into the final polymeric network.

Rigid zeolite containing polyurethane foams

DOEpatents

Frost, C.B.

1984-05-18

A closed cell rigid polyurethane foam has been prepared which contains up to about 60% by weight of molecular sieves capable of sorbing molecules with effective critical diameters of up to about 10 A. The molecular sieve component of the foam can be preloaded with catalysts or with reactive compounds that can be released upon activation of the foam to control and complete crosslinking after the foam is formed. The foam can also be loaded with water or other flame-retarding agents, after completion. Up to about 50% of the weight of the isocyanate component of the foam can be replaced by polyimide resin precursors for incorporation into the final polymeric network.

High-Glass-Transition-Temperature Polyimides Developed for Reusable Launch Vehicle Applications

NASA Technical Reports Server (NTRS)

Chuang, Kathy; Ardent, Cory P.

2002-01-01

Polyimide composites have been traditionally used for high-temperature applications in aircraft engines at temperatures up to 550 F (288 C) for thousands of hours. However, as NASA shifts its focus toward the development of advanced reusable launch vehicles, there is an urgent need for lightweight polymer composites that can sustain 600 to 800 F (315 to 427 C) for short excursions (hundreds of hours). To meet critical vehicle weight targets, it is essential that one use lightweight, high-temperature polymer matrix composites in propulsion components such as turbopump housings, ducts, engine supports, and struts. Composite materials in reusable launch vehicle components will heat quickly during launch and reentry. Conventional composites, consisting of layers of fabric or fiber-reinforced lamina, would either blister or encounter catastrophic delamination under high heating rates above 300 C. This blistering and delamination are the result of a sudden volume expansion within the composite due to the release of absorbed moisture and gases generated by the degradation of the polymer matrix. Researchers at the NASA Glenn Research Center and the Boeing Company (Long Beach, CA) recently demonstrated a successful approach for preventing this delamination--the use of three-dimensional stitched composites fabricated by resin infusion.

In-Plane Shear Testing of Medium and High Modulus Woven Graphite Fiber Reinforced/Polyimide Composites

NASA Technical Reports Server (NTRS)

Gentz, M.; Armentrout, D.; Rupnowski, P.; Kumosa, L.; Shin, E.; Sutter, J. K.; Kumosa, M.

2004-01-01

Iosipescu shear tests were performed at room temperature and at 316 C (600 F) o woven composites with either M40J or M60J graphite fibers and PMR-II-50 polyimide resin matrix. The composites were tested as supplied and after thermo-cycling, with the thermo-cycled composites being tested under dry and wet conditions. Acoustic emission (AE) was monitored during the room and high temperature Iosipescu experiments. The shear stresses at the maximum loads and the shear stresses at the significant onset of AE were determined for the composites as function of temperature and conditioning. The combined effects of thermo-cycling and moisture on the strength and stiffness properties of the composites were evaluated. It was determined that the room and high temperature shear stresses at the maximum loads were unaffected by conditioning. However, at room temperature the significant onset of AE was affected by conditioning; the thermal conditioned wet specimens showed the highest shear stress at the onset of AE followed by thermal-conditioned and then as received specimens. Also, at igh temperature the significant onset of AE occurred in some specimens after the maximum load due to the viscoelastoplastic nature of the matrix material.

Processing and Characterization of Carbon Nanotube Composites

NASA Technical Reports Server (NTRS)

Can, Roberto J.; Grimsley, Brian W.; Czabaj, Michael W.; Siochi, Emilie J.; Hull, Brandon

2014-01-01

Recent advances in the synthesis of large-scale quantities of carbon nanotubes (CNT) have provided the opportunity to study the mechanical properties of polymer matrix composites using these novel materials as reinforcement. Nanocomp Technologies, Inc. currently supplies large sheets with dimensions up to 122 cm x 244 cm containing both single-wall and few-wall CNTs. The tubes are approximately 1 mm in length with diameters ranging from 8 to 12 nm. In the present study being conducted at NASA Langley Research Center (LaRC), single and multiple layers of CNT sheets were infused or coated with various polymer solutions that included commercial toughened-epoxies and bismaleimides, as well as a LaRC developed polyimide. The resulting CNT composites were tested in tension using a modified version of ASTM D882-12 to determine their strength and modulus values. The effects of solvent treatment and mechanical elongation/alignment of the CNT sheets on the tensile performance of the composite were determined. Thin composites (around 50 wt% CNT) fabricated from acetone condensed and elongated CNT sheets with either a BMI or polyimide resin solution exhibited specific tensile moduli approaching that of toughened epoxy/ IM7 carbon fiber unidirectional composites.

Immobilization of long-lived radionuclides in carbon matrices produced with the use of polyimide binders

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abdulakhatov, Murat; Bartenev, Sergey; Firsin, Nikolai

Available in abstract form only. Full text of publication follows: Conditions for immobilization of long-lived radionuclides {sup 99}Tc, {sup 129}I and {sup 241}Am in carbon matrices were investigated by using their chemical analogs. Stable isotopes of rhenium, iodine and europium were used as chemical analogs of {sup 99}Tc, {sup 129}I and {sup 241}Am, respectively. It is shown that the carbon matrices incorporating the above elements can be produced by carbonization of composites with ITA-31 polyimide binder of the following composition: equal molar ratio between dianhydride of 3,3/,4,4/-benzophenone-tetracarboxylic acid and tetraacetyl derivative of 4,4/-diaminodiphenyl ester, radionuclide being investigated or its chemicalmore » analog and carbon fabric as reinforcing component. The elements under investigation were used both in the form of salts or oxides and in the form of their complexes with ion-exchange resins. The produced composites were carbonized in inert gas (argon) or in vacuum. The physical-chemical properties of the samples were studied. It was revealed that the resultant matrices meet the requirements imposed on waste storage and final disposal. (authors)« less

77 FR 63288 - Proposed Information Collection; Comment Request; Manufacturers' Unfilled Orders Survey

Federal Register 2010, 2011, 2012, 2013, 2014

2012-10-16

... need for periodic benchmarking of the M3 estimates to reflect the manufacturing universe. The Annual.... The Census Bureau will use these data to develop universe estimates of unfilled orders as of the end...

Kinetics and mechanics of photo-polymerized triazole-containing thermosetting composites via the copper(I)-catalyzed azide-alkyne cycloaddition

PubMed Central

Song, Han Byul; Wang, Xiance; Patton, James R.; Stansbury, Jeffrey W.; Bowman, Christopher N.

2017-01-01

Objectives Several features necessary for polymer composite materials in practical applications such as dental restorative materials were investigated in photo-curable CuAAC (copper(I)-catalyzed azide-alkyne cycloaddition) thermosetting resin-based composites with varying filler loadings and compared to a conventional BisGMA/TEGDMA based composite. Methods Tri-functional alkyne and di-functional azide monomers were synthesized for CuAAC resins and incorporated with alkyne-functionalized silica microfillers for CuAAC composites. Polymerization kinetics, in situ temperature change, and shrinkage stress were monitored simultaneously with a tensometer coupled with FTIR spectroscopy and a data-logging thermocouple. The glass transition temperature was analyzed by dynamic mechanical analysis. Flexural modulus/strength and flexural toughness were characterized in three-point bending on a universal testing machine. Results The photo-CuAAC polymerization of composites containing between 0 and 60 wt% microfiller achieved ~99% conversion with a dramatic reduction in the maximum heat of reaction (~20 °C decrease) for the 60 wt% filled CuAAC composites as compared with the unfilled CuAAC resin. CuAAC composites with 60 wt% microfiller generated more than twice lower shrinkage stress of 0.43±0.01 MPa, equivalent flexural modulus of 6.1±0.7 GPa, equivalent flexural strength of 107±9 MPa, and more than 10 times higher energy absorption of 10±1 MJ m−3 when strained to 11% relative to BisGMA-based composites at equivalent filler loadings. Significance Mechanically robust and highly tough, photo-polymerized CuAAC composites with reduced shrinkage stress and a modest reaction exotherm were generated and resulted in essentially complete conversion. PMID:28363645

Kinetics and mechanics of photo-polymerized triazole-containing thermosetting composites via the copper(I)-catalyzed azide-alkyne cycloaddition.

PubMed

Song, Han Byul; Wang, Xiance; Patton, James R; Stansbury, Jeffrey W; Bowman, Christopher N

2017-06-01

Several features necessary for polymer composite materials in practical applications such as dental restorative materials were investigated in photo-curable CuAAC (copper(I)-catalyzed azide-alkyne cycloaddition) thermosetting resin-based composites with varying filler loadings and compared to a conventional BisGMA/TEGDMA based composite. Tri-functional alkyne and di-functional azide monomers were synthesized for CuAAC resins and incorporated with alkyne-functionalized glass microfillers for CuAAC composites. Polymerization kinetics, in situ temperature change, and shrinkage stress were monitored simultaneously with a tensometer coupled with FTIR spectroscopy and a data-logging thermocouple. The glass transition temperature was analyzed by dynamic mechanical analysis. Flexural modulus/strength and flexural toughness were characterized in three-point bending on a universal testing machine. The photo-CuAAC polymerization of composites containing between 0 and 60wt% microfiller achieved ∼99% conversion with a dramatic reduction in the maximum heat of reaction (∼20°C decrease) for the 60wt% filled CuAAC composites as compared with the unfilled CuAAC resin. CuAAC composites with 60wt% microfiller generated more than twice lower shrinkage stress of 0.43±0.01MPa, equivalent flexural modulus of 6.1±0.7GPa, equivalent flexural strength of 107±9MPa, and more than 10 times higher energy absorption of 10±1MJm -3 when strained to 11% relative to BisGMA-based composites at equivalent filler loadings. Mechanically robust and highly tough, photo-polymerized CuAAC composites with reduced shrinkage stress and a modest reaction exotherm were generated and resulted in essentially complete conversion. Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Demineralization of resin-sealed enamel by soft drinks in a clinically relevant pH cycling model.

PubMed

Bartels, Agata A; Evans, Carla A; Viana, Grace; Bedran-Russo, Ana K

2016-04-01

To compare the in vitro protective effect of orthodontic sealants on the enamel demineralization under a soft drink-induced erosive challenge. The facial surfaces of bovine incisors were sectioned into 5 mm x 4 mm x 4 mm enamel blocks. Specimens were randomly assigned to three surface protection measures: control (exposed enamel), coating with Transbond XT (unfilled resin primer), or coating with Opal Seal (filled and fluoride releasing primer). Thermocycling was used to simulate aging. The specimens were pH cycled through an acidic buffer, test beverage and a neutral buffer for a total of 7 days. Test beverages included water, Diet Mountain Dew, and Coke Classic. Quantitative light-induced fluorescence (QLF) images were taken at baseline and after aging. Final QLF images were taken to evaluate the demineralization of enamel. Data were analyzed statistically using a two-way ANOVA to compare the interaction between enamel surface protection and beverages as well as one-way ANOVA to compare surface protection and the test beverage levels. A statistically significant interaction was found between the surface protected groups and the test beverage groups (P < 0.05). Statistically significant differences were found among the test beverage groups (P < 0.05) and among the surface protection groups (P < 0.05). Coke Classic went through the sealant layer resulting in high enamel demineralization. Enamel coating with Opal Seal significantly reduced the erosive attack of beverages.

Mechanical Properties of LaRC(tm) SI Polymer for a Range of Molecular Weights

NASA Technical Reports Server (NTRS)

Whitley, Karen S.; Gates, Thomas S.; Hinkley, Jeffrey A.; Nicholson, Lee M.

2000-01-01

Mechanical testing of an advanced polyimide resin (LaRC(tm)-SI) with known variations in molecular weight was performed over a range of temperatures below the glass transition temperature. Elastic and inelastic properties were characterized as a function of molecular weight and test temperature. It was shown that notched tensile strength is a strong function of both temperature and molecular weight, whereas stiffness is only a strong function of temperature. The combined analysis of calculated yield stress and notched tensile strength indicated that low molecular weight materials tended to fail in a brittle manner, whereas high molecular weight materials exhibited ductile failure. The microphotographs of the failure surfaces also supported these findings.

Comparison of Graphite Fabric Reinforced PMR-15 and Avimid N Composites After Long Term Isothermal Aging at Various Temperatures

NASA Technical Reports Server (NTRS)

Bowles, Kenneth J.; McCorkle, Linda; Ingrahm, Linda

1998-01-01

Extensive effort is currently being expended to demonstrate the feasibility of using high-performance, polymer-matrix composites as engine structural materials over the expected operating lifetime of the aircraft, which can extend from 18,000 to 30,000 hr. The goal is to develop light-weight, high-strength, and high-modulus materials for use in higher temperature sections of advanced 21 st century aircraft propulsion systems. To accomplish this goal, it is necessary to pursue the development of thermal and mechanical durability models for graphite-fiber-reinforced, polymer-matrix composites. Numerous investigations have been reported regarding the thermo-oxidative stability (TOS) of the polyimide PMR-15 (1-5). A significant amount of this work has been directed at edge and geometry effects, reinforcement fiber influences, and empirical modeling of high-temperature weight loss behavior. It is yet to be determined if the information obtained from the PMR-15 composite tests is applicable to other polyimide-matrix composites. The condensation-curing polymer Avimid N is another advanced composite material often considered for structural applications at high temperatures. Avimid N has better thermo-oxidative stability than PMR-15 (6), but the latter is more easily processed. The most comprehensive study of the thermo-oxidative stability of Avimid N neat resin and composites at 371 (infinity)C is found in Salin and Seferis (7). The purposes of the work described herein were to compare the thermal aging behavior of these two matrix polymers and to determine the reasons for and the consequences of the difference in thermal durability. These results might be of some use in improving future polymer development through the incorporation of the desirable characteristics of both polyimides.

Study of improved resins for advanced supersonic technology composites. Part 1: Heteroaromatic polymers containing ether groups. Part 2: Curing chemistry of aromatic polymers and composite studies

NASA Technical Reports Server (NTRS)

Takekoshi, T.; Hillig, W. B.; Mellinger, G. A.

1975-01-01

Fourteen ether-containing, aromatic dianhydrides have been synthesized from N-phenyl-3 or 4-nitrophthalimide and various bisphenols. The process involves nucleophilic displacement of activated nitro groups with bisphenolate ions. Ether-containing dianhydrides were indefinitely stable in the presence of atmospheric moisture. One-step, high temperature solution polymerization of the ether-containing dianhydrides with m-phenylene diamine, 4,4'-oxydianiline and 1, 3-bis(4-aminophenoxy)benzene afforded 42 polyetherimides. The polyetherimides were all soluble in m-cresol except two which were found to be crystalline. The glass transition temperatures of the polyetherimides ranged from 178 to 277 C. Soluble polybenzimidazopyrrolones containing ether groups were also prepared from the same ether-containing dianhydrides and aromatic tetraamines by one-step solution polymerization. Using low molecular weight polyetherimides, various thermoset resin systems were developed and tested as matrices for fiber-reinforced composites. The curing chemistry involving reaction of the phthalonitrile group and the o-diaminophenyl group was found to be generally applicable to crosslinking various aromatic polymers other than polyimides.

Final Report: Research Study on Development of Environmental Friendly Spray-on Foam Insulation (SOFI) for the External Tank (ET)

NASA Technical Reports Server (NTRS)

Stuckey, James M.

1996-01-01

The selection and quantification of four foams using a more environmentally friendly HCFC-141b blowing agent replacing foams that used the CFC-11 blowing agent for the external tank (ET) LWT has been addressed along with problems and solutions that were encountered during verification. The effort on two lower density spray foams for the ET SLWT are presented, but predicted weight savings were not encouraging. Suggestions for possible problem solving are included along with a new approach for selecting foams for qualification as back-up foams for the foams used on the ET LWT. We investigated three resins for use as thermally sprayed coatings for corrosion prevention on metal. The best coating was obtained with a thermoplastic polyimide resin. This coating has a good chance of meeting ET requirements. Possible third generation blowing agents have been shown usable in polyurethane spray and pour foams, and solubility in isocyannate foam components are acceptable. We considered aerogels as insulation materials on space vehicles, and suggested a liner for a liquid oxygen (LOX) composite tank.

Investigation of Mild Steel Thin-Wall Tubes in Unfilled and Foam-Filled Triangle, Square, and Hexagonal Cross Sections Under Compression Load

NASA Astrophysics Data System (ADS)

Rajak, Dipen Kumar; Kumaraswamidhas, L. A.; Das, S.

2018-02-01

This study has examined proposed structures with mild steel-reinforced LM30 aluminum (Al) alloy having diversely unfilled and 10 wt.% SiCp composite foam-filled tubes for improving axial compression performance. This class of material has novel physical, mechanical, and electrical properties along with low density. In the present experiment, Al alloy foams were prepared by the melt route technique using metal hydride powder as a foaming agent. Crash energy phenomena for diverse unfilled and foam-filled in mild steel thin-wall tubes (triangular, square and hexagonal) were studied as well. Compression deformation investigation was conducted at strain rates of 0.001-0.1/s for evaluating specific energy absorption (SEA) under axial loading conditions. The results were examined to measure plateau stress, maximum densification strain, and deformation mechanism of the materials. Specific energy absorption and total energy absorption capacities of the unfilled and filled sections were determined from the compressive stress-strain curves, which were then compared with each other.

Mechanical Properties of T650-35/AFR-PE-4 at Elevated Temperatures for Lightweight Aeroshell Designs

NASA Technical Reports Server (NTRS)

Whitley, Karen S.; Collins, TImothy J.

2006-01-01

Considerable efforts have been underway to develop multidisciplinary technologies for aeroshell structures that will significantly increase the allowable working temperature for the aeroshell components, and enable the system to operate at higher temperatures while sustaining performance and durability. As part of these efforts, high temperature polymer matrix composites and fabrication technologies are being developed for the primary load bearing structure (heat shield) of the spacecraft. New high-temperature resins and composite material manufacturing techniques are available that have the potential to significantly improve current aeroshell design. In order to qualify a polymer matrix composite (PMC) material as a candidate aeroshell structural material, its performance must be evaluated under realistic environments. Thus, verification testing of lightweight PMC's at aeroshell entry temperatures is needed to ensure that they will perform successfully in high-temperature environments. Towards this end, a test program was developed to characterize the mechanical properties of two candidate material systems, T650-35/AFR-PE-4 and T650-35/RP46. The two candidate high-temperature polyimide resins, AFR-PE-4 and RP46, were developed at the Air Force Research Laboratory and NASA Langley Research Center, respectively. This paper presents experimental methods, strength, and stiffness data of the T650-35/AFR-PE-4 material as a function of elevated temperatures. The properties determined during the research test program herein, included tensile strength, tensile stiffness, Poisson s ratio, compressive strength, compressive stiffness, shear modulus, and shear strength. Unidirectional laminates, a cross-ply laminate and two eight-harness satin (8HS)-weave laminates (4-ply and 10-ply) were tested according to ASTM standard methods at room and elevated temperatures (23, 316, and 343 C). All of the relevant test methods and data reduction schemes are outlined along with mechanical data. These data contribute to a database of material properties for high-temperature polyimide composites that will be used to identify the material characteristics of potential candidate materials for aeroshell structure applications.

Experimental evaluation and design of unfilled and concrete-filled FRP composite piles : Task 4A : design specifications.

DOT National Transportation Integrated Search

2015-08-01

The overall goal of this project is the experimental evaluation and design of unfilled and concrete-filled FRP composite piles for load-bearing in bridges. This report covers Task 4A, Design Specifications. : Structural design specifications are base...

Microleakage and penetration depth of different fissure sealant materials after cyclic thermo-mechanic and brushing simulation.

PubMed

Hatirli, Hüseyin; Yasa, Bilal; Yasa, Elif

2018-01-30

The aim of the study was to evaluate microleakage and the penetration-depths of different fissure-sealant materials applied with/without enameloplasty after cyclic aging. One-hundred-sixty mandibular molars were divided into non-invasive and enameloplasty preparation groups and eight material subgroups, including: flowable composites (microhyrid, nanohybrid, and nanofilled), three resin-based (unfilled, filled, and highly-filled), a giomer-based, and a glass-ionomer-based fissure sealant. Specimens were subjected to two-year cyclic chewing and brushing simulation. After 5% basic-fuchsin dye penetration, specimens were sectioned and scored under stereomicroscope. Kruskal-Wallis statistical data showed that preparation type significantly affected the penetration of all tested materials (p<0.05), but not significantly affected microleakage (p>0.05). Flowable composites showed the best and the glass-ionomer-based sealant showed the worst penetration and microleakage. Slight preparation of fissures is not important in microleakage. However, enameloplasty significantly enhanced the depth of penetration of the sealants. Flowable composites offer promising results at the fissure sealing.

Fabrication of polyimide based microfluidic channels for biosensor devices

NASA Astrophysics Data System (ADS)

Zulfiqar, Azeem; Pfreundt, Andrea; Svendsen, Winnie Edith; Dimaki, Maria

2015-03-01

The ever-increasing complexity of the fabrication process of Point-of-care (POC) devices, due to high demand of functional versatility, compact size and ease-of-use, emphasizes the need of multifunctional materials that can be used to simplify this process. Polymers, currently in use for the fabrication of the often needed microfluidic channels, have limitations in terms of their physicochemical properties. Therefore, the use of a multipurpose biocompatible material with better resistance to the chemical, thermal and electrical environment, along with capability of forming closed channel microfluidics is inevitable. This paper demonstrates a novel technique of fabricating microfluidic devices using polyimide (PI) which fulfills the aforementioned properties criteria. A fabrication process to pattern microfluidic channels, using partially cured PI, has been developed by using a dry etching method. The etching parameters are optimized and compared to those used for fully cured PI. Moreover, the formation of closed microfluidic channel on wafer level by bonding two partially cured PI layers or a partially cured PI to glass with high bond strength has been demonstrated. The reproducibility in uniformity of PI is also compared to the most commonly used SU8 polymer, which is a near UV sensitive epoxy resin. The potential applications of PI processing are POC and biosensor devices integrated with microelectronics.

Manufacture and mechanical characterisation of high voltage insulation for superconducting busbars - (Part 1) Materials selection and development

NASA Astrophysics Data System (ADS)

Clayton, N.; Crouchen, M.; Devred, A.; Evans, D.; Gung, C.-Y.; Lathwell, I.

2017-04-01

It is planned that the high voltage electrical insulation on the ITER feeder busbars will consist of interleaved layers of epoxy resin pre-impregnated glass tapes ('pre-preg') and polyimide. In addition to its electrical insulation function, the busbar insulation must have adequate mechanical properties to sustain the loads imposed on it during ITER magnet operation. This paper reports an investigation into suitable materials to manufacture the high voltage insulation for the ITER superconducting busbars and pipework. An R&D programme was undertaken in order to identify suitable pre-preg and polyimide materials from a range of suppliers. Pre-preg materials were obtained from 3 suppliers and used with Kapton HN, to make mouldings using the desired insulation architecture. Two main processing routes for pre-pregs have been investigated, namely vacuum bag processing (out of autoclave processing) and processing using a material with a high coefficient of thermal expansion (silicone rubber), to apply the compaction pressure on the insulation. Insulation should have adequate mechanical properties to cope with the stresses induced by the operating environment and a low void content necessary in a high voltage application. The quality of the mouldings was assessed by mechanical testing at 77 K and by the measurement of the void content.

Experimental evaluation and design of unfilled and concrete-filled FRP composite piles : Task 4B : material & construction specifications : final report.

DOT National Transportation Integrated Search

2015-07-01

The overall goal of this project is the experimental evaluation and design of unfilled and concrete-filled FRP composite piles for load-bearing in bridges. This report covers Task 4B, Materials and Construction Specifications. : This technical report...

77 FR 65666 - Correction: Proposed Information Collection; Comment Request; Manufacturers' Unfilled Orders Survey

Federal Register 2010, 2011, 2012, 2013, 2014

2012-10-30

... DEPARTMENT OF COMMERCE U.S. Census Bureau Correction: Proposed Information Collection; Comment Request; Manufacturers' Unfilled Orders Survey AGENCY: U.S. Census Bureau, Commerce. ACTION: Correction. SUMMARY: On October 16, 2012, a notice was published in the Federal Register (77 FR 63288) on the proposed...

Experimental evaluation and design of unfilled and concrete-filled FRP composite piles, task 3 - FRP composite pile flexural testing.

DOT National Transportation Integrated Search

2014-06-01

The overall goal of this project is the experimental evaluation and design of unfilled and concrete-filled FRP : composite piles for load-bearing in bridges. This report covers Task 3, FRP Composite Pile Flexural Testing. : Hollow and concrete filled...

Experimental evaluation and design of unfilled and concrete-filled FRP composite piles, task 6 - FRP composite pile axial compression testing.

DOT National Transportation Integrated Search

2015-04-01

The overall goal of this project is the experimental evaluation and design of unfilled and concrete-filled FRP : composite piles for load-bearing in bridges. This report covers Task 6, FRP Composite Pile Axial Compression : Testing. : Hollow and conc...

Experimental evaluation and design of unfilled and concrete-filled FRP composite piles : Task 7 : final report : thesis.

DOT National Transportation Integrated Search

2015-05-01

The overall goal of this project is the experimental evaluation and design of unfilled and concrete-filled FRP composite piles for load-bearing in bridges. This report covers Task 7, Final Report - Thesis. : This final report covers Tasks 1, 2, 3, 5 ...

Experimental evaluation and design of unfilled and concrete-filled FRP composite piles : Task 5 : laminate durability testing : final report.

DOT National Transportation Integrated Search

2015-05-01

The overall goal of this project is the experimental evaluation and design of unfilled and concrete-filled FRP composite piles for load-bearing in bridges. This report covers Task 5, Laminate Durability Testing. : Mechanical properties of the FRP mat...

Experimental evaluation and design of unfilled and concrete-filled FRP composite piles, task 1 - mechanical properties of FRP piles.

DOT National Transportation Integrated Search

2014-10-01

The overall goal of this project is the experimental evaluation and design of unfilled and concrete-filled FRP : composite piles for load-bearing in bridges. This report covers Task 1, Mechanical Properties of FRP Piles. : Mechanical and geotechnic...

Selection and Manufacturing of Membrane Materials for Solar Sails

NASA Technical Reports Server (NTRS)

Bryant, Robert G.; Seaman, Shane T.; Wilkie, W. Keats; Miyaucchi, Masahiko; Working, Dennis C.

2013-01-01

Commercial metallized polyimide or polyester films and hand-assembly techniques are acceptable for small solar sail technology demonstrations, although scaling this approach to large sail areas is impractical. Opportunities now exist to use new polymeric materials specifically designed for solar sailing applications, and take advantage of integrated sail manufacturing to enable large-scale solar sail construction. This approach has, in part, been demonstrated on the JAXA IKAROS solar sail demonstrator, and NASA Langley Research Center is now developing capabilities to produce ultrathin membranes for solar sails by integrating resin synthesis with film forming and sail manufacturing processes. This paper will discuss the selection and development of polymer material systems for space, and these new processes for producing ultrathin high-performance solar sail membrane films.

17 CFR 1.48 - Requirements for classification of sales or purchases for future delivery as bona fide hedging of...

Code of Federal Regulations, 2010 CFR

2010-04-01

... classification of sales or purchases for future delivery as bona fide hedging of unsold anticipated production or... for future delivery as bona fide hedging of unsold anticipated production or unfilled anticipated... anticipated production or unfilled anticipated requirements described in these statements shall not be...

Condensation polyimides

NASA Technical Reports Server (NTRS)

Hergenrother, P. M.

1989-01-01

Polyimides belong to a class of polymers known as polyheterocyclics. Unlike most other high temperature polymers, polyimides can be prepared from a variety of inexpensive monomers by several synthetic routes. The glass transition and crystalline melt temperature, thermooxidative stability, toughness, dielectric constant, coefficient of thermal expansion, chemical stability, mechanical performance, etc. of polyimides can be controlled within certain boundaries. This versatility has permitted the development of various forms of polyimides. These include adhesives, composite matrices, coatings, films, moldings, fibers, foams and membranes. Polyimides are synthesized through both condensation (step-polymerization) and addition (chain growth polymerization) routes. The precursor materials used in addition polyimides or imide oligomers are prepared by condensation method. High molecular weight polyimide made via polycondensation or step-growth polymerization is studied. The various synthetic routes to condensation polyimides, structure/property relationships of condensation polyimides and composite properties of condensation polyimides are all studied. The focus is on the synthesis and chemical structure/property relationships of polyimides with particular emphasis on materials for composite application.

Fillers for improved graphite fiber retention by polymer matrix composites

NASA Technical Reports Server (NTRS)

House, E. E.; Sheppard, C. H.

1981-01-01

The results of a program designed to determine the extent to which elemental boron and boron containing fillers added to the matrix resin of graphite/epoxy composites prevent the release of graphite fibers when the composites are exposed to fire and impact conditions are described. The fillers evaluated were boron, boron carbide and aluminum boride. The conditions evaluated were laboratory simulations of those that could exist in the event of an aircraft crash and burn situation. The baseline (i.e., unfilled) laminates evaluated were prepared from commercially available graphite/epoxy. The baseline and filled laminates' mechanical properties, before and after isothermal and humidity aging, also were compared. It was found that a small amount of graphite fiber was released from the baseline graphite/epoxy laminates during the burn and impact conditions used in this program. However, the extent to which the fibers were released is not considered a severe enough problem to preclude the use of graphite reinforced composites in civil aircraft structure. It also was found that the addition of boron and boron containing fillers to the resin matrix eliminated this fiber release. Mechanical properties of laminates containing the boron and boron containing fillers were lower than those of the baseline laminates. These property degradations for two systems: boron (5 micron) at 2.5 percent filler loading, and boron (5 micron) at 5.0 percent filler loading do not appear severe enough to preclude their use in structural composite applications.

Microshear bond strength of self-etching systems associated with a hydrophobic resin layer.

PubMed

De Vito Moraes, André Guaraci; Francci, Carlos; Carvalho, Ceci Nunes; Soares, Silvio Peixoto; Braga, Roberto Ruggiero

2011-08-01

To evaluate in vitro the microshear bond strength of adhesive systems applied to dentin according to manufacturers' instructions, associated or not with a hydrophobic layer of unfilled resin. Six self-etching adhesives (Clearfil SE Bond, Kuraray Medical; AdheSE, Ivoclar Vivadent; Xeno III, Dentsply; I Bond, Heraeus-Kulzer; Bond Force, Tokuyama; Futurabond DC, Voco) were tested. The labial dentin of sixty bovine incisors was exposed, and the teeth were divided into two groups according to the application or not of an extra hydrophobic resin layer (Scotchbond Multi Purpose Plus, bottle 3). Six composite cylinders (Filtek Z250, 3M ESPE) were built up on each treated surface. Specimens were stored in distilled water at 37ºC for 24 h and then subjected to the microshear bond strength test in a universal testing machine at a crosshead speed of 0.5 mm/min. Microshear bond strength values were analyzed by 2-way ANOVA and Tukey's post-hoc test. Failure mode was determined using a stereomicroscope under 20X magnification. The application of the hydrophobic resin layer did not affect bond strength, except for AdheSE. However, the bond strengths with the hydrophobic layer were similar among the six tested systems (Clearfil: 17.1 ± 7.9; AdheSE: 14.5 ± 7.1; Xeno lll: 12.8 ± 7.7; I Bond: 9.5 ± 5.8; Bond Force: 17.5 ± 4.1; Futurabond: 7.7 ± 2.3). When used as recommended by the manufacturers, Bond Force presented statistically higher bond strength than AdheSE and I Bond (p < 0.05) (Clearfil 10.4 ± 4.9; AdheSE 1.6 ± 1.6; Xeno lll: 9.0 ± 3.8; I Bond: 3.0 ± 1.5; Bond Force: 14 ± 3.9; Futurabond: 8.8 ± 3.8). Failure mode was predominantly adhesive. The bond strength of the self-etching systems tested was not significantly affected by the application of a hydrophobic layer, but a significant improvement was observed in AdheSE.

Experimental evaluation and design of unfilled and concrete-filled FRP composite piles, task 2 - FRP composite pile driving at the Richmond-Dresden bridge over the Kennebec River.

DOT National Transportation Integrated Search

2014-01-01

The overall goal of this project is the experimental evaluation and design of unfilled and concrete-filled FRP : composite piles for load-bearing in bridges. This report covers Task 2, FRP Composite Pile Driving at the : Richmond-Dresden Bridge over ...

Processing and properties of fiber reinforced polymeric matrix composites: I. IM7/LARC(TM)-PETI-7 polyimide composites

NASA Technical Reports Server (NTRS)

Hou, Tan-Hung

1995-01-01

A phenylethynyl terminated imide oligomer formed from the reaction of benzophenone tetracarboxylic acid dianhydride, an 75:25 molar ratio of 4,4'-oxydianiline and meta-phenylenediamine and 4-phenylethynylphthalic anhydride as the endcapper at a theoretical number average molecular weight (Mn) of approximately 3,700 g/mol was evaluated as a composite resin matrix. A glass transition temperature (Tg) of 315 deg C was reached after 250 deg C/1 hr annealing of the matrix resin. Unidirectional prepreg was made by coating an N-methylpyrrolidinone solution of the amide acid oligomer onto unsized IM7 graphite fibers. The thermal and rheological properties and the solvent/volatile depletion rates of the amide acid/NMP system were determined. This information was used to successfully design a molding cycle for composite fabrication. Composites molded under 800 Psi at 371 C consistently yielded good consolidation as measured by C-scan and optical photomicrography. The composite's short beam shear strength (SBS), longitudinal and transverse flexural strengths and moduli were measured at various temperatures. These composites exhibited excellent room temperature (RT) longitudinal flexural strength and modulus and RT SBS strength retention at 177 C.

An improved compression molding technology for continuous fiber reinforced composite laminate. Part 1: AS-4/LaRC-TPI 1500 (HFG) Prepreg system

NASA Technical Reports Server (NTRS)

Hou, Tan-Hung; Kidder, Paul W.; Reddy, Rakasi M.

1991-01-01

Poor processability of fiber reinforced high performance polyimide thermoplastic resin composites is a well recognized issue which, in many cases, prohibits the fabrication of composite parts with satisfactorily consolidated quality. Without modifying the resin matrix chemistry, improved compression modeling procedures were proposed and investigated with the AS-4/LaRC-TPI 1500 High Flow Grade (HFG) prepreg system. Composite panels with excellent C-scans can be consistently molded by this method under 700 F and a consolidation pressure as low as 100 psi. A mechanism for the consolidation of the composite under this improved molding technique is discussed. This mechanism reveals that a certain degree of matrix shear and tow filament slippage and nesting between plies occur during consolidation, which leads to a reduction of the consolidating pressure necessary to offset the otherwise intimate inter fiber-fiber contact and consequently achieves a better consolidation quality. Outstanding short beam shear strength and flexural strength were obtained from the molded panels. A prolonged consolidation step under low pressure, i.e., 100 psi at 700 F for 75 minutes, was found to significantly enhance the composite mechanical properties.

PMR polyimide composites for aerospace applications. [Polymerization of Monomer Reactants

NASA Technical Reports Server (NTRS)

Serafini, T. T.

1984-01-01

A novel class of addition-type polyimides has been developed in response to the need for high temperature polymers with improved processability. The new plastic materials are known as PMR (for in situ polymerization of monomer reactants) polyimides. The highly processable PMR polyimides have made it possible to realize much of the potential of high temperature resistant polymers. Monomer reactant combinations for several PMR polyimides have been identified. The present investigation is concerned with a review of the current status of PMR polyimides. Attention is given to details of PMR polyimide chemistry, the processing of composites and their properties, and aerospace applications of PMR-15 polyimide composites.

Area-selective atomic layer deposition of platinum using photosensitive polyimide.

PubMed

Vervuurt, René H J; Sharma, Akhil; Jiao, Yuqing; Kessels, Wilhelmus Erwin M M; Bol, Ageeth A

2016-10-07

Area-selective atomic layer deposition (AS-ALD) of platinum (Pt) was studied using photosensitive polyimide as a masking layer. The polyimide films were prepared by spin-coating and patterned using photolithography. AS-ALD of Pt using poly(methyl-methacrylate) (PMMA) masking layers was used as a reference. The results show that polyimide has excellent selectivity towards the Pt deposition, after 1000 ALD cycles less than a monolayer of Pt is deposited on the polyimide surface. The polyimide film could easily be removed after ALD using a hydrogen plasma, due to a combination of weakening of the polyimide resist during Pt ALD and the catalytic activity of Pt traces on the polyimide surface. Compared to PMMA for AS-ALD of Pt, polyimide has better temperature stability. This resulted in an improved uniformity of the Pt deposits and superior definition of the Pt patterns. In addition, due to the absence of reflow contamination using polyimide the nucleation phase during Pt ALD is drastically shortened. Pt patterns down to 3.5 μm were created with polyimide, a factor of ten smaller than what is possible using PMMA, at the typical Pt ALD processing temperature of 300 °C. Initial experiments indicate that after further optimization of the polyimide process Pt features down to 100 nm should be possible, which makes AS-ALD of Pt using photosensitive polyimide a promising candidate for patterning at the nanoscale.

Large-Strain Transparent Magnetoactive Polymer Nanocomposites

NASA Technical Reports Server (NTRS)

Meador, Michael A.

2012-01-01

A document discusses polymer nano - composite superparamagnetic actuators that were prepared by the addition of organically modified superparamagnetic nanoparticles to the polymer matrix. The nanocomposite films exhibited large deformations under a magnetostatic field with a low loading level of 0.1 wt% in a thermoplastic polyurethane elastomer (TPU) matrix. The maximum actuation deformation of the nanocomposite films increased exponentially with increasing nanoparticle concentration. The cyclic deformation actuation of a high-loading magnetic nanocomposite film was examined in a low magnetic field, and it exhibited excellent reproducibility and controllability. Low-loading TPU nanocomposite films (0.1-2 wt%) were transparent to semitransparent in the visible wavelength range, owing to good dispersion of the magnetic nanoparticles. Magnetoactuation phenomena were also demonstrated in a high-modulus, high-temperature polyimide resin with less mechanical deformation.

On the radiation tolerance of SU-8, a new material for gaseous microstructure radiation detector fabrication

NASA Astrophysics Data System (ADS)

Key, M. J.; Cindro, V.; Lozano, M.

2004-12-01

SU-8 photosensitive epoxy resin was developed for the fabrication of high-aspect ratio microstructures in MEMS and microengineering applications, and has potential for use in the construction of novel gaseous micropattern radiation detectors. However, little is known of the behaviour of the cured material under irradiation. Mechanical properties of SU-8 film have been measured as a function of neutron exposure and compared with Kapton ® polyimide and Mylar ® PET polyester films, materials routinely used in gaseous radiation detectors, to asses the suitability of SU-8 based microstructures for gaseous detector applications. After exposure to a reactor core neutron fluence of 7.5×10 18 n cm -2, the new material showed a high level of resistance to radiation damage, comparable to Kapton film.

Composite seals for liquid hydrogen and nuclear radiation environments.

NASA Technical Reports Server (NTRS)

Van Auken, R. L.; Chase, V. A.

1971-01-01

Description of plastic composite seals for service in a liquid-hydrogen and nuclear-radiation environment. The radiation-resistant aromatic heterocyclic class of polymers, including polyimide, polybenzimidazole, and polyquinoxaline, were evaluated for this application. The seal developed is based on a design involving a resin-starved laminate consisting of alternating layers of woven glass fabric and polymer film. This design imparts a mechanical spring characteristic to the seal, resulting in essentially complete elastic recovery when unloaded, and eliminates cold flow. Encapsulating techniques employing the polyquinoxaline polymer were developed which rendered the seal impervious to liquid hydrogen. The seals were tested before and after gamma irradiation up to 10 to the 10th ergs/g. Load/deflection and leakage tests were performed over a temperature range from -423 through +500 F.

Negative birefringent polyimide films

NASA Technical Reports Server (NTRS)

Harris, Frank W. (Inventor); Cheng, Stephen Z. D. (Inventor)

1994-01-01

A negative birefringent film, useful in liquid crystal displays, and a method for controlling the negative birefringence of a polyimide film is disclosed which allows the matching of an application to a targeted amount of birefringence by controlling the degree of in-plane orientation of the polyimide by the selection of functional groups within both the diamine and dianhydride segments of the polyimide which affect the polyimide backbone chain rigidity, linearity, and symmetry. The higher the rigidity, linearity and symmetry of the polyimide backbone, the larger the value of the negative birefringence of the polyimide film.

Tribological properties at 25 C of seven polyimide films bonded to 440 C high-temperature stainless steel

NASA Technical Reports Server (NTRS)

Fusaro, R. L.

1982-01-01

The tribological properties of seven polyimide films applied to 440 C high temperature stainless steel substrates were studied at 25 C with a pin-on-disk type of friction and were apparatus. The polyimides fell into two groups according to friction and wear properties. Group I polyimides had slightly lower friction but much higher wear than group II polyimides. The wear mechanism was predominately adhesion, but the wear particles were larger for group I polyimides. For most of the polyimides the transfer films consisted of clumps of compacted wear particles. One polyimide composition produced a very thin transfer film that sheared plastically in the contact area.

Evaluation of different types of enamel conditioning before application of a fissure sealant.

PubMed

Ciucchi, Philip; Neuhaus, Klaus W; Emerich, Marta; Peutzfeldt, Anne; Lussi, Adrian

2015-01-01

The aim of the study was to compare fissure sealant quality after mechanical conditioning of erbium-doped yttrium aluminium garnet (Er:YAG) laser or air abrasion prior to chemical conditioning of phosphoric acid etching or of a self-etch adhesive. Twenty-five permanent molars were initially divided into three groups: control group (n = 5), phosphoric acid etching; test group 1 (n = 10), air abrasion; and test group 2, (n = 10) Er:YAG laser. After mechanical conditioning, the test group teeth were sectioned buccolingually and the occlusal surface of one half tooth (equal to one sample) was acid etched, while a self-etch adhesive was applied on the other half. The fissure system of each sample was sealed, thermo-cycled and immersed in 5% methylene dye for 24 h. Each sample was sectioned buccolingually, and one slice was analysed microscopically. Using specialized software microleakage, unfilled margin, sealant failure and unfilled area proportions were calculated. A nonparametric ANOVA model was applied to compare the Er:YAG treatment with that of air abrasion and the self-etch adhesive with phosphoric acid (α = 0.05). Test groups were compared to the control group using Wilcoxon rank sum tests (α = 0.05). The control group displayed significantly lower microleakage but higher unfilled area proportions than the Er:YAG laser + self-etch adhesive group and displayed significantly higher unfilled margin and unfilled area proportions than the air-abrasion + self-etch adhesive group. There was no statistically significant difference in the quality of sealants applied in fissures treated with either Er:YAG laser or air abrasion prior to phosphoric acid etching, nor in the quality of sealants applied in fissures treated with either self-etch adhesive or phosphoric acid following Er:YAG or air-abrasion treatment.

Toughening elastomers with sacrificial bonds and watching them break.

PubMed

Ducrot, Etienne; Chen, Yulan; Bulters, Markus; Sijbesma, Rint P; Creton, Costantino

2014-04-11

Elastomers are widely used because of their large-strain reversible deformability. Most unfilled elastomers suffer from a poor mechanical strength, which limits their use. Using sacrificial bonds, we show how brittle, unfilled elastomers can be strongly reinforced in stiffness and toughness (up to 4 megapascals and 9 kilojoules per square meter) by introducing a variable proportion of isotropically prestretched chains that can break and dissipate energy before the material fails. Chemoluminescent cross-linking molecules, which emit light as they break, map in real time where and when many of these internal bonds break ahead of a propagating crack. The simple methodology that we use to introduce sacrificial bonds, combined with the mapping of where bonds break, has the potential to stimulate the development of new classes of unfilled tough elastomers and better molecular models of the fracture of soft materials.

Polyimide Precursor Solid Residuum

NASA Technical Reports Server (NTRS)

Weiser, Erik S. (Inventor); St.Clair, Terry L. (Inventor); Echigo, Yoshiaki (Inventor); Kaneshiro, Hisayasu (Inventor)

2001-01-01

A polyimide precursor solid residuum is an admixture of an aromatic dianhydride or derivative thereof and an aromatic diamine or derivative thereof plus a complexing agent, which is complexed with the admixture by hydrogen bonding. The polyimide precursor solid residuum is effectively employed in the preparation of polyimide foam and the fabrication of polyimide foam structures.

Review of Polyimides Used in the Manufacturing of Micro Systems

NASA Technical Reports Server (NTRS)

Wilson, William C.; Atkinson, Gary M.

2007-01-01

Since their invention, polyimides have found numerous uses in MicroElectroMechanical Systems (MEMS) technology. Polyimides can act as photoresist, sacrificial layers, structural layers, and even as a replacement for silicon as the substrate during MEMS fabrication. They enable fabrication of both low and high aspect ratio devices. Polyimides have been used to fabricate expendable molds and reusable flexible molds. Development of a variety of devices that employ polyimides for sensor applications has occurred. Micro-robotic actuator applications include hinges, thermal actuators and residual stress actuators. Currently, polyimides are being used to create new sensors and devices for aerospace applications. This paper presents a review of some of the many uses of polyimides in the development of MEMS devices, including a new polyimide based MEMS fabrication process.

Relationship between Training Programs being Offered in State and Federal Penal Institutions and the Unfilled Job Openings in the Major Occupations in the United States.

ERIC Educational Resources Information Center

Torrence, John Thomas

Excluding military installations, training programs in state and federal penal institutions were surveyed, through a mailed checklist, to test the hypotheses that (1) training programs in penal institutions were not related to the unfilled job openings by major occupations in the United States, and (2) that training programs reported would have a…

Fundamental aspects of polyimide dry film and composite lubrication: A review

NASA Technical Reports Server (NTRS)

Fusaro, R. L.

1982-01-01

The tribological properties of polyimide dry films and composites are reviewed. Friction coefficients, wear rates, transfer film characteristics, wear surface morphology, and possible wear mechanisms of several different polyimide films, polyimide-bonded solid lubricants, polyimide solid bodies, and polyimide composites are discussed. Such parameters as temperature, type of atmosphere, load, contact stress, and specimen configuration are investigated. Data from an accelerated test device (Pin-on-Disk) are compared to similar data obtained from an end use application test device (plain spherical bearing).

Semi-interpenetrating polymer network's of polyimides: Fracture toughness

NASA Technical Reports Server (NTRS)

Hansen, Marion Glenn

1988-01-01

The objective was to improve the fracture toughness of the PMR-15 thermosetting polyimide by co-disolving LaRC-TPI, a thermoplastic polyimide. The co-solvation of a thermoplastic into a thermoset produces an interpenetration of the thermoplastic polymer into the thermoset polyimide network. A second research program was planned around the concept that to improve the fracture toughness of a thermoset polyimide polymer, the molecular weight between crosslink points would be an important macromolecular topological parameter in producing a fracture toughened semi-IPN polyimide.

Correlating the synthesis protocol of aromatic polyimide film with the properties of polyamic acid precursor

NASA Astrophysics Data System (ADS)

Tan, P. C.; Ooi, B. S.; Ahmad, A. L.; Low, S. C.

2017-06-01

Thousands of different copolyimide combinations render it technically impossible to have a single universal synthesis method to produce aromatic polyimide film. This study aimed to outline the selection of synthesis protocol, either through the casting of chemically imidized polyimide solution or thermal imidization of polyamic acid (PAA), to produce the polyimide film. The rheological behaviour, molecular weight, and solubility of five structurally different PAA were analysed and correlated to both imidization methods. In this work, a tough polyimide film was successfully synthesized by casting the chemically imidized polyimide derived from high viscosity (> 81 cP) and high molecular weight (≥ 1.35 x 106 g/mol) PAA. On the contrary, both low viscosity (< 13 cP) and high viscosity (> 81 cP) PAA demonstrated the possibility to produce polyimide film via thermal imidization route. The longer molecular chain of ODPA-6FpDA:DABA (3:2) polyimide produced from thermal imidization had restricted the passage of CO2 across the polyimide film when it was applied in the gas separation application. The outcome from this work serves as a guideline for the selection of suitable polyimide film synthesis protocol, which will minimize the time and chemical consumption in future exploration of new polyimide structure.

Polyimides Containing Fluorine and Phosphorus for Potential Space Applications

NASA Technical Reports Server (NTRS)

Connell, John W.; Watson, Kent A.

2000-01-01

As part of an effort to develop low color, ultraviolet (UV) radiation and atomic oxygen resistant polyimides for potential space applications, a novel diamine containing fluorine and phosphorus was synthesized and used to prepare polyimides. The approach was to combine attributes from colorless, UV resistant polyimides and atomic oxygen (AO) resistant polymers into a single material. Preparation of colorless polyimides has focused on minimization of charge transfer complex formation by incorporation of bulky substituents and disrupting conjugation by using meta-catenated monomers. AO resistant polymer technology development has focused on placing phenylphosphine oxide groups into the backbone of aromatic polymers. However, polyimides prepared utilizing this approach thus far have all exhibited significant color. Thus in an attempt to combine these features in a polyimide a new diamine, bis(3-aminophenyl)-3,5-di(trifluoromethyl)phenylphosphine oxide (TFMDA) was synthesized and used to prepare polyimides. The polyimides were cast into films and characterized for physical and mechanical properties, optical transmission and AO and UV resistance.

A comparison of the effects of toothbrushing and handpiece prophylaxis on retention of sealants.

PubMed

Kolavic Gray, Shellie; Griffin, Susan O; Malvitz, Dolores M; Gooch, Barbara F

2009-01-01

Tooth surface cleaning before acid etching is considered to be an important step in the retention of resin-based pit-and-fissure sealants. The authors reviewed and summarized instructions for cleaning tooth surfaces from five manufacturers of 10 unfilled resin-based sealants marketed in the United States. The authors also searched electronic databases for studies that directly compared the effects of different surface-cleaning methods on sealant retention and for systematic reviews of the effectiveness of sealants. They explored the association between surface-cleaning methods and sealant retention in the studies included in the systematic reviews. They calculated the summary weighted retention rates for studies that used either a handpiece or toothbrush prophylaxis. All of the sealant manufacturers' instructions for use (IFU) recommended cleaning the tooth before acid etching. None of the IFU directly stated that a handpiece was required to perform the cleaning, but five IFU implied the use of handpiece prophylaxis. None of the IFU recommended surface-altering procedures in caries-free teeth. Direct evidence from two clinical trials showed no difference in complete sealant retention between surfaces cleaned mechanically with pumice or prophylaxis paste and those cleaned with air-water syringe or dry toothbrushing. Indirect evidence from 10 studies found that weighted summary retention by year after sealant placement in studies that used toothbrush prophylaxis was greater than or equivalent to values for studies that used handpiece prophylaxis. Levels of sealant retention after surface cleaning with toothbrush prophylaxis were at least as high as those associated with hand-piece prophylaxis. This finding may translate into lower resource costs for sealant placement.

Antimicrobial and biological activity of leachate from light curable pulp capping materials.

PubMed

Arias-Moliz, Maria Teresa; Farrugia, Cher; Lung, Christie Y K; Wismayer, Pierre Schembri; Camilleri, Josette

2017-09-01

Characterization of a number of pulp capping materials and assessment of the leachate for elemental composition, antimicrobial activity and cell proliferation and expression. Three experimental light curable pulp-capping materials, Theracal and Biodentine were characterized by scanning electron microscopy, energy dispersive spectroscopy and X-ray diffraction. The elemental composition of the leachate formed after 24h was assessed by inductively coupled plasma (ICP). The antimicrobial activity of the leachate was determined by the minimum inhibitory concentration (MIC) against multispecies suspensions of Streptococcus mutans ATCC 25175, Streptococcus gordonii ATCC 33478 and Streptococcus sobrinus ATCC 33399. Cell proliferation and cell metabolic function over the material leachate was assessed by an indirect contact test using 3-(4,5 dimethylthiazolyl-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay. The hydration behavior of the test materials varied with Biodentine being the most reactive and releasing the highest amount of calcium ions in solution. All materials tested except the unfilled resin exhibited depletion of phosphate ions from the solution indicating interaction of the materials with the media. Regardless the different material characteristics, there was a similar antimicrobial activity and cellular activity. All the materials exhibited no antimicrobial activity and were initially cytotoxic with cell metabolic function improving after 3days. The development of light curable tricalcium silicate-based pulp capping materials is important to improve the bonding to the final resin restoration. Testing of both antimicrobial activity and biological behavior is critical for material development. The experimental light curable materials exhibited promising biological properties but require further development to enhance the antimicrobial characteristics. Copyright © 2017 Elsevier Ltd. All rights reserved.

In vitro fracture resistance of roots obturated with epoxy resin-based, mineral trioxide aggregate-based, and bioceramic root canal sealers.

PubMed

Topçuoğlu, Hüseyin Sinan; Tuncay, Öznur; Karataş, Ertuğrul; Arslan, Hakan; Yeter, Kübra

2013-12-01

The aim of this study was to evaluate the fracture resistance of teeth filled with 3 different endodontic sealers. Seventy-five single-rooted extracted mandibular premolars were decoronated to a length of 13 mm. The teeth were randomly divided into 5 groups (n = 15 for each group). In group 1, the teeth were left unprepared and unfilled (negative control), and in group 2, the teeth were left unobturated (positive control). The rest of the roots were prepared by using the ProTaper System up to a master apical file size of F3: group 3, bioceramic sealer (Endosequence BC sealer) + gutta-percha; group 4, mineral trioxide aggregate-based sealer (Tech Biosealer Endo) + gutta-percha; and group 5, epoxy resin-based sealer (AH Plus Jet) + gutta-percha. All root specimens were stored for 2 weeks at 100% humidity to allow the complete setting of the sealers. Each specimen was then subjected to fracture testing by using a universal testing machine at a crosshead speed of 1.0 mm/min(-1) until the root fractured. The force required to fracture each specimen was recorded, and the data were analyzed statistically. The fracture values of groups 3 and 5 were significantly higher than those of group 4 (P < .05). There was no significant difference between groups 3 and 5 (P > .05). In contrast to Tech Biosealer Endo, Endosequence BC and AH Plus Jet sealer increased the force to fracture in root-filled single-rooted premolar teeth. Copyright © 2013 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

Property evolution during vitrification of dimethacrylate photopolymer networks

PubMed Central

Abu-Elenain, Dalia; Lewis, Steven H.; Stansbury, Jeffrey W.

2013-01-01

Objectives This study seeks to correlate the interrelated properties of conversion, shrinkage, modulus and stress as dimethacrylate networks transition from rubbery to glassy states during photopolymerization. Methods An unfilled BisGMA/TEGDMA resin was photocured for various irradiation intervals (7–600 s) to provide controlled levels of immediate conversion, which was monitored continuously for 10 min. Fiber optic near-infrared spectroscopy permitted coupling of real-time conversion measurement with dynamic polymerization shrinkage (linometer), modulus (dynamic mechanical analyzer) and stress (tensometer) development profiles. Results The varied irradiation conditions produced final conversion ranging from 6 % to more than 60 %. Post-irradiation conversion (dark cure) was quite limited when photopolymerization was interrupted either at very low or very high levels of conversion while significant dark cure contributions were possible for photocuring reactions suspended within the post-gel, rubbery regime. Analysis of conversion-based property evolution during and subsequent to photocuring demonstrated that the shrinkage rate increased significantly at about 40 % conversion followed by late-stage suppression in the conversion-dependent shrinkage rate that begins at about 45–50 % conversion. The gradual vitrification process over this conversion range is evident based on the broad but well-defined inflection in the modulus versus conversion data. As limiting conversion is approached, modulus and, to a somewhat lesser extent, stress rise precipitously as a result of vitrification with the stress profile showing little if any late-stage suppression as seen with shrinkage. Significance Near the limiting conversion for this model resin, the volumetric polymerization shrinkage rate slows while an exponential rise in modulus promotes the vitrification process that appears to largely dictate stress development. PMID:24080378

New Materials for the Repair of Polyimide Electrical Wire Insulation

NASA Technical Reports Server (NTRS)

2008-01-01

Two viable polyimide backbone materials have been identified that will allow the repair of polyimide electrical wire insulation found on the Space Shuttle and other aging aircraft. This identification is the outcome of ongoing efforts to assess the viability of using such polyimides and polyimide precursors (polyamic acids [PAAs]) as repair materials for aging polyimide electrical wire insulation. These repair materials were selected because they match the chemical makeup of the underlying wire insulation as closely as possible. This similarity allows for maximum compatibility, coupled with the outstanding physical properties of polyimides. The two polyimide backbone materials allow the polymer to be extremely flexible and to melt at low temperatures. A polymer chain end capping group that allows the polymer to crosslink into a nonflowable repair upon curing at around 200 C was also identified.

Reactive Additives for Phenylethynyl-Containing Resins

NASA Technical Reports Server (NTRS)

Connell, John W.; Smith, Joseph G., Jr.; Hergenrother, Paul M.; Rommel, Monica L.

2005-01-01

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.

Polyimides formulated from a partially fluorinated diamine for aerospace tribological applications

NASA Technical Reports Server (NTRS)

Fusaro, R. L.

1983-01-01

Preliminary tribological studies on polyimides formulated from the diamine 2,2-bis 4-(4-aminophenoxy)phenyl hexafluorapane (4-BDAF) indicate that polyimides formulated from this diamine have excellent potential for high temperature tribological applications. The dianhydrides used to make the polyimides were pyromellitic (PMDA) and benzophenonetetracarboxylic acid (BTDA). Friction and wear studies at 25 and 200 C indicate that polyimides formulated using 50 mole percent of the PMDA dianhydride and 50 mole percent of the BTDA dianhydride perform better than polyimides formulated solely with the BTDA dianhydride. Graphite fiber reinforced polyimide composites were formulated with the polyimide made from the BTDA dianhydride, both graphitic and non-graphitic fibers were evaluated. Graphitic fibers produced better tribological results, since thin, flowing, "layer-like' transfer films were produced which did not build-up with long sliding durations. Non-graphitic fibers did not produce this type of transfer.

PMR polyimide composites for aerospace applications

NASA Technical Reports Server (NTRS)

Serafini, T. T.

1982-01-01

Fiber reinforced PMR polyimides are finding increased acceptance as engineering materials for high performance structural applications. Prepreg materials based on this novel class of highly processable, high temperature resistant polyimides, are commercially available and the PMR concept was incorporated in several industrial applications. The status of PMR polyimides is reviewed. Emphasis is given to the chemistry, processing, and applications of the first generation PMR polyimides known as PMR-15.

Analytical research and development for the Whitney Programs. Automation and instrumentation. Computer automation of the Cary Model 17I spectrophotometer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Haugen, G.R.; Bystroff, R.I.; Downey, R.M.

1975-09-01

In the area of automation and instrumentation, progress in the following studies is reported: computer automation of the Cary model 17I spectrophotometer; a new concept for monitoring the concentration of water in gases; on-line gas analysis for a gas circulation experiment; and count-rate-discriminator technique for measuring grain-boundary composition. In the area of analytical methodology and measurements, progress is reported in the following studies: separation of molecular species by radiation pressure; study of the vaporization of U(thd)$sub 4$, (thd = 2,2,6,6-tetramethylheptane-3,5-drone); study of the vaporization of U(C$sub 8$H$sub 8$)$sub 2$; determination of ethylenic unsaturation in polyimide resins; and, semimicrodetermination of hydroxylmore » and amino groups with pyromellitic dianhydride (PMDA). (JGB)« less

Development of a highly reliable composite board for printed circuitry for use in space environment

NASA Technical Reports Server (NTRS)

Bradbury, E. J.; Markle, R. A.; Dunnavant, W. R.; Stickney, P. B.

1971-01-01

Materials, processes and fabrication techniques have been investigated for the development of a high-temperature circuit-board laminate. High quality, void-free copper-clad laminates have been made using 7628/HS-1 style fiberglas reinforcements with filled polyimide matrices. The fabricating characteristics of P13N resin appear suitable for use as a filled matrix in this circuit board development. High-fired, ball-milled alumina appears to be necessary to obtain the desired effects in the circuit board system. Nickel-clad copper foil bonding surfaces appear to be another requirement for retention of good bond strengths after art work and plating sequences. The fabrication cycle for this circuit board system is very dependent on the heating profile. Very rapid heating with quick loading is recommended. A stack approach to lamination was successfully used.

Structure/permeability relationships of silicon-containing polyimides

NASA Technical Reports Server (NTRS)

Stern, S. A.; Vaidyanathan, R.; Pratt, J. R.

1989-01-01

The permeability to H2, O2, N2, CO2 and CH4 of three silicone-polyimide random copolymers and two polyimides containing silicon atoms in their backbone chains, was determined at 35.0 C and at pressures up to about 120 psig (approximately 8.2 atm). The copolymers contained different amounts of BPADA-m-PDA and amine-terminated poly (dimethyl siloxane) and also had different numbers of siloxane linkages in their silicone component. The polyimides containing silicon atoms (silicon-modified polyimides) were SiDA-4,4'-ODA and SiDA-p-PDA. The gas permeability and selectivity of the copolymers are more similar to those of their silicone component than of the polyimide component. By contrast, the permeability and selectivity of the silicon-modified polyimides are more similar to those of their parent polyimides, PMDA-4,4'-ODA and SiDA-p-PDA. The substitution of SiDA for the PMDA moiety in a polyimide appears to result in a significant increase in gas permeability, without a correspondingly large decrease in selectivity. The potential usefulness of the above polymers and copolymers as gas separation membranes is discussed.

Photomechanical Deformation of Azobenzene-Functionalized Polyimides Synthesized with Bulky Substituents (Postprint)

DTIC Science & Technology

2017-12-06

mechanical response of the azobenzene- functionalized polyimide is correlated to the rotational freedom of the polyimide chains (resulting in extensive... correlated to the rotational freedom of the polyimide chains (resulting in extensive segmental mobility) and fractional free volume (FFV > 0.1...response has been described,34 and a recent simulation study on the stress relaxation dynamics of azo-polyimides has provided insights into the correlation

Polyimides containing amide and perfluoroisopropylidene connecting groups

NASA Technical Reports Server (NTRS)

Dezern, James F. (Inventor)

1993-01-01

New, thermooxidatively stable polyimides were prepared from the reaction of aromatic dianhydrides containing isopropylidene bridging groups with aromatic diamines containing amide connecting groups between the rings. Several of these polyimides were shown to be semi-crystalline as evidenced by wide angle x ray scattering and differential scanning calorimetry. Most of the polyimides form tough, flexible films with high tensile properties. These polyimide films exhibit enhanced solubility in organic solvents.

Polyimides containing pendent siloxane groups

NASA Technical Reports Server (NTRS)

Connell, John W. (Inventor); St.clair, Terry L. (Inventor); Hergenrother, Paul M. (Inventor)

1994-01-01

Novel polyimides containing pendent siloxane groups (PISOX) were prepared by the reaction of functionalized siloxane compounds with hydroxy containing polyimides (PIOH). The pendent siloxane groups on the polyimide backbone offer distinct advantages such as lowering the dielectric constant and moisture resistance and enhanced atomic oxygen resistance. The siloxane containing polyimides are potentially useful as protective silicon oxide coatings and are useful for a variety of applications where atomic oxygen resistance is needed.

Systems and methods for using a boehmite bond-coat with polyimide membranes for gas separation

DOEpatents

Polishchuk, Kimberly Ann

2013-03-05

The subject matter disclosed herein relates to gas separation membranes and, more specifically, to polyimide gas separation membranes. In an embodiment, a gas separation membrane includes a porous substrate, a substantially continuous polyimide membrane layer, and one or more layers of boehmite nanoparticles disposed between the porous substrate and the polyimide membrane layer to form a bond-coat layer. The bond-coat layer is configured to improve the adhesion of the polyimide membrane layer to the porous substrate, and the polyimide membrane layer has a thickness approximately 100 nm or less.

Anchoring energy of photo-sensitive polyimide alignment film containing methoxy cinnamate

NASA Astrophysics Data System (ADS)

Kim, Suyoung; Shin, Sung Eui; Shin, DongMyung

2010-02-01

Photosensitive polyimide containing 2-methoxy cinnamate was synthesized for photo-alignment layer of liquid crystals (LCs). 2-Methoxy cinnamic acid was confirmed photo-sensitive material by linearly polarized UV light. We studied that effect of polarized UV light on rubbed polyimide film. Anchoring energy of liquid crystal with aligning surface was measured. Irradiation of depolarized UV light on rubbed Polyimide film suppressed effective anchoring energy. Linearly polarized UV light on rubbed polyimide film controlled anchoring energy effectively. Polyimide film containing 2-methoxy cinnamate can control the photo-alignment layer easily due to its photo-sensitivity.

Space Survivability of Main-Chain and Side-Chain POSS-Kapton Polyimides

NASA Astrophysics Data System (ADS)

Tomczak, Sandra J.; Wright, Michael E.; Guenthner, Andrew J.; Pettys, Brian J.; Brunsvold, Amy L.; Knight, Casey; Minton, Timothy K.; Vij, Vandana; McGrath, Laura M.; Mabry, Joseph M.

2009-01-01

Kapton® polyimde (PI) is extensively used in solar arrays, spacecraft thermal blankets, and space inflatable structures. Upon exposure to atomic oxygen (AO) in low Earth orbit (LEO), Kapton® is severely degraded. An effective approach to prevent this erosion is chemically bonding polyhedral oligomeric silsesquioxane (POSS) into the polyimide matrix by copolymerization of POSS-diamine with the polyimide monomers. POSS is a silicon and oxygen cage-like structure surrounded by organic groups and can be polymerizable. The copolymerization of POSS provides Si and O in the polymer matrix on the nano level. During POSS polyimide exposure to atomic oxygen, organic material is degraded and a silica passivation layer is formed. This silica layer protects the underlying polymer from further degradation. Ground-based studies and MISSE-1 and MISSE-5 flight results have shown that POSS polyimides are resistant to atomic-oxygen attack in LEO. In fact, 3.5 wt% Si8O11 main-chain POSS polyimide eroded about 2 μm during the 3.9 year flight in LEO, whereas 32 μm of 0 wt% POSS polyimide would have eroded within 4 mos. The atomic-oxygen exposure of main-chain POSS polyimides and new side-chain POSS polyimides has shown that copolymerized POSS imparts similar AO resistance to polyimide materials regardless of POSS monomer structure.

The effects of long-duration space exposure on the mechanical properties of some carbon-reinforced resin matrix composites

NASA Technical Reports Server (NTRS)

Vyhnal, Richard F.

1993-01-01

Long Duration Exposure Facility (LDEF) Experiment A0175 involved the non-instrumented exposure of seven carbon-fiber reinforced resin-matrix advanced composite panels contained in two trays - A7 and A1. These two trays were located, respectively, on the leading and trailing faces of LDEF, obliquely oriented to the RAM (Row 9) and WAKE (Row 3) directions. The identity and location of the seven panels, which consisted of six flat laminates of the following material systems are shown: carbon/epoxy (T300/934), carbon/bismaleimide (T300/F178), and carbon/polyimide (C6000/LARC-160 and C6000/PMR-15), plus one bonded honeycomb sandwich panel (T300/934 face sheets and Nomex core) patterned after the Space Shuttle payload bay door construction. These material systems were selected to represent a range of then-available matrix resins which, by virtue of their differing polymer chemistry, could conceivably exhibit differing susceptibility to the low-earth orbit (LEO) environment. The principal exposure conditions of the LDEF environment at these tray locations are shown. Noteworthy to some of the observations discussed is the four-orders-of magnitude difference in the atomic oxygen (AO) fluence, which made a shallow incidence angle (approximately 22 deg) to Tray A7, while Tray A1 on the trailing face was essentially shielded from AO exposure. This evaluation focused on determining the individual and relative suitability of a variety of resin-matrix composite systems for long-term space structural applications. This was accomplished primarily by measuring and comparing a range of engineering mechanical properties on over 300 test coupons sectioned from the flight panels and from identical control panels, and tested at ambient and elevated temperatures. This testing was supported by limited physical characterization, involving visual examination of flight panel surface features, measurements of weight loss and warpage, and examination for changes in internal integrity (micro cracking, delamination) by ultrasonic c-scan and polished cross-sections.

Polyimides from 2,3,3',4'-Biphenyltetracarboxylic Dianhydride and Aromatic Diamines

NASA Technical Reports Server (NTRS)

Hergenrother, Paul M. (Inventor); Smith, Joseph G. (Inventor); Connell, John W. (Inventor); Watson, Kent A. (Inventor)

2005-01-01

The present invention relates generally to polyimides. It relates particularly to novel polyimides prepared from 2,3, 3',4' -biphenyltetracarboxylic dianhydride and aromatic diamines. These novel polyimides have low color, good solubility, high thermal emissivity, low solar absorptivity and high tensile strength.

Photodegradation of Polyimides 2. Thermal Property Changes of Polyimides Based on a Perfluorinated Dianhydride

DTIC Science & Technology

1989-05-31

BASED Ck ON A PERFLUORINATED DIANHYDRIDE a (𔃾 by i C. E. Hoyle and E. T. Anzures Prepared for Publicatlon in J. Appl. olym. Sci. SDTIC ELECTE...34Photodegradation of Polyimides 2. Thermal Property Changes of Polyimides Based on a Perfluorinated Dianhydride" 12. PERSONAL AUTHOR(S) C. E. Hoyle and E...Additionally, the glass transition of photolyzed of polyimides containing the perfluorinated moiety is lowered with increasing photolysis time. By

Property enchancement of polyimide films by way of the incorporation of lanthanide metal ions

NASA Technical Reports Server (NTRS)

Thompson, David W.

1993-01-01

Lanthanide metal ions were incorporated into the polyimide derived from 2,2-bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride (6FDA) and 1,3-bis(aminophenoxy) benzene (APB) in an attempt to produce molecular level metal-polymer composites. The lanthanide series of metal ions (including aluminum, scandium, and yttrium) provide discrete and stable metal ions in the 3+ oxidation state. Throughout the series there is a uniform variation in ionic size ranging from 50 pm for aluminum to a maximum of 103.4 pm for cerium and gradually decreasing again to 84.8 pm for lutetium. The high charge-to-size ratio for these ions as well as the ability to obtain large coordination numbers makes them excellent candidates for interacting with the polymer substructure. The distinct lack of solubility of simple lanthanide salts such as the acetates and halides has made it difficult to obtain metal ions distributed in the polymer framework as discrete ions or metal complexes rather than microcomposites of metal clusters. (Lanthanum nitrates are quite soluble, but the presence of the strongly oxidizing nitrate ion leads to serious degradation of the polymer upon thermal curing. This work was successful at extending the range of soluble metals salts by using chelating agents derived from the beta-diketones dipivaloylmethane, dibenzoylmethane, trifluoroacetylacetone, and hexafluoroacetylacetone. Metal acetates which are insoluble in dimethylacetamide dissolve readily in the presence of the diketones. Addition of the polyimide yields a homogeneous resin which is then cast into a clear film. Upon curing clear films were obtained with the dibenzoylmethane and trifluoroacetylacetone ligands. The dipavaloylmethane precipitates the metal during the film casting process, and hexafluoroacetylacetone gives cured films which are deformed and brittle. These clear films are being evaluated for the effect of the metal ions on the coefficient of thermal expansion, resistance to atomic oxygen, and on selective gas permeability. Much more commonly than above, polyimide films are prepared by casting the film as the poly(amic acid) precursor which is then converted to the imidized form during the thermal cure cycle. Very limited success was achieved in the past in adding lanthanide metal ions to the amide precursors because of gellation and lack of solubility. With the use of the diketone ligands cited above, the solubility and gellation problems were overcome. However, the films after curing were clear but unacceptably brittle. Attempts to overcome this cure embrittlement problem are in progress.

Improving DLA Aviation Engineering’s Support to its Customers and the DoD Supply Chain

DTIC Science & Technology

2014-10-01

costs and first article test costs) and (2) DLA supply chain responsiveness as measured in terms of the days required to satisfy unfilled orders ( UFOs ...135,000 UFOs or requisitions at any time. This number of UFOs overstates the magnitude of the backorder problem since many of these backorders are...backorders or long term unfilled orders ( UFOs ). This can have serious implications for the materiel readiness of those weapon systems that utilize

Crosslinked polyimides prepared from N-(3-ethynylphenyl)maleimide

NASA Technical Reports Server (NTRS)

Gerber, Margaret K. (Inventor); St.clair, Terry L. (Inventor)

1993-01-01

The compound N-(3-ethynylphenyl)maleimide (NEPMI) was used to prepare thermally stable, glassy polyimides which did not exhibit glass transition temperatures below 500 C. NEPMI was blended with the maleimide of methylene dianiline (BMI) and heated to form the polyimide. NEPMI was also mixed with Thermid 600 R, a commercially available bisethynyl oligomeric material, and heated to form a thermally stable, glassy polyimide. Lastly, NEPMI was blended with both BMI and Thermid 600 R to form thermally stable, glassy polyimides.

Development of an impact- and solvent-resistant thermoplastic composite matrix

NASA Technical Reports Server (NTRS)

Delano, C. B.; Kiskiras, C. J.

1984-01-01

Synthesis, moldability and chloroform, acetone and tricresyl phosphate resistance of 16 polymer compositions are described. These aliphatic heterocyclic polymers include polyimides, polybenzimidazoles, and N-arylenepolybenzimidazoles. A solution condensation (cresol) method to prepare imidized aliphaic polyimides is described. Two polyimides and one polybenzimidazole demonstrate no crazing or cracking during 500 hr exposure to the cited solvents under stress. Modification of one aliphatic polyimide with several aromatic amines suggests that m-phenylenediamine is singular in its behavior to improve the chloroform resistance of that class of polyimides.

Polyimide Film of Increased Tear Strength

NASA Technical Reports Server (NTRS)

St. Clair, A. K.; Hinkley, J. A.; Ezzell, S. A.

1986-01-01

High-temperature linear aromatic polyimide with improved resistance to tearing made by new process that incorporates elastomer into polyimide. Linear aromatic condensation polyimides are materials of prime choice for use as films and coatings on advanced spacecraft and aircraft where durability at temperatures in range of 200 to 300 degree C required. Elastomer-containing polyimide film with improved toughness proves useful for applications where resistance to tearing and long-term thermal stability necessary. Desired resistance to tearing achieved by careful control of amount and chemical composition of added elastomer.

Photodegradation of Polyimide 1. A Spectral, Viscometric, Chromatographic and Weight Loss Investigation of Polyimides Based on a Perfluorinated Dianhydride

DTIC Science & Technology

1989-05-31

A SPECTRAL, VISC’)METRIC, CHROMATOGRAPHIC AND WEIGHT LOSS INVESTIGATION OF POLYIMIDES BASED ON A PERFLUORINATED DIANHYDRIDE by C. E. Hoyle and E. T...and Weight Loss Investigation of Polyimides Based on a Perfluorinated Dianhyd c A2. PERSONAL AUTHOR(S) C. E. Hoyle and E. T. Anzures 13a. TYPE OF REPORT...polyimide films with perfluorinated chromophores in the dianhydride moiety is characterized by significant weight loss and chain cleavage. A conventional

Tin-polyimide and indium-polyimide thin-film composites as soft X-ray bandpass filters

NASA Technical Reports Server (NTRS)

Powell, Stephen F.; Allen, Maxwell J.; Willis, Thomas D.

1993-01-01

A tin-polyimide and an indium-polyimide soft X-ray bandpass filter were fabricated with thicknesses of 1400 and 1750 A for the metal and polyimide components, respectively. The transmission of each filter was measured at the Stanford Synchrotron Radiation Laboratory. The transmission of the tin-polyimide filter was found to be about 40 percent for radiation with wavelengths between 60 and 80 A. The transmission of the indium-polyimide filter was greater than 40 percent between 70 and 90 A. The indium was about 5 percent more transmissive than the tin and attained a maximum transmission of about 48 percent at 76 A. Such filters have potential applications to soft X-ray telescopes that operate in this region. They might also be of interest to investigators who work with X-ray microscopes that image live biological specimens in the 23-44-A water window.

Low wear partially fluorinated polyimides

NASA Technical Reports Server (NTRS)

Fusaro, R. L.; Hady, W. F.

1984-01-01

Tribological studies were conducted on five different polyimide solid bodies formulated from the diamine 2,2-bis 4-(4-aminophenoxy)phenyl hexafluoropropane (4-BDAF) and the dianhydrides pyromellitic acid (PMDS) and benzophenonetetracarboxylic acid (BTDA). The following polyimides were evaluated 4-BDAF/PMDA, 4-BDAF/BTDA, 4-BDAF/80 mole percent PMDA, 20 mole percent BTDA, 4-BDAF/60 mole percent BTDA. Friction coefficients, polyimide wear rates, polyimide surface morphology and transfer films were evaluated at sliding speeds of 0.31 to 11.6 m/s and at temperatures of 25 C to 300 C. The results indicate that the tribological properties are highly dependent on the composition of the polyimide and on the experimental conditions. Two polyimides were found which produced very low wear rates but very high friction coefficients (greater than 0.85) under ambient conditions. They offer considerable potential for high traction types of application such as brakes.

Methyl substituted polyimides containing carbonyl and ether connecting groups

NASA Technical Reports Server (NTRS)

Hergenrother, Paul M. (Inventor); Havens, Stephen J. (Inventor)

1992-01-01

Polyimides were prepared from the reaction of aromatic dianhydrides with novel aromatic diamines having carbonyl and ether groups connecting aromatic rings containing pendant methyl groups. The methyl substituent polyimides exhibit good solubility and form tough, strong films. Upon exposure to ultraviolet irradiation and/or heat, the methyl substituted polyimides crosslink to become insoluble.

Stripping and splicing polyimide-coated fibers

NASA Astrophysics Data System (ADS)

Duke, Douglas; Kanda, Yoshiharu; Tobita, Kenyo; Yamauchi, Ryozo

2011-05-01

Polyimide is often used as a coating material for optical fibers used in high temperature environments such as aerospace or oil and gas sensor applications. Unfortunately, polyimide coating is very difficult to strip by conventional mechanical stripping methods. The glass fiber is easily damaged if the stripping process is not extremely well controlled. Stripping the polyimide coating by heating with a flame or arc typically results in a significant reduction in fiber strength. Strength may be maintained by using hot acid stripping, however the use of the strong hot acid presents safety hazards and also requires controlled and safe waste disposal. Another issue with polyimide coating is variability of the coating diameter from various manufacturers or due to different polyimide coating processes. This not only complicates the polyimide stripping issue, but also presents problems with precise clamping and alignment during splicing, especially when it is necessary to splice with a short cleave length. In this paper, we present new polyimide coating stripping technology. The significant feature of this stripping technology is achievement of good strength while avoiding the use of hot acid or heating. We also developed a new specialty fiber fusion splicer that enables precise alignment and splicing regardless of the variability of polyimide coating diameter, even when clamping on the coating.

Structure-property study of keto-ether polyimides

NASA Technical Reports Server (NTRS)

Dezern, James F.; Croall, Catharine I.

1991-01-01

As part of an on-going effort to develop an understanding of how changes in the chemical structure affect polymer properties, an empirical study was performed on polyimides containing only ether and/or carbonyl connecting groups in the polymer backbone. During the past two decades the structure-property relationships in linear aromatic polyimides have been extensively investigated. More recently, work has been performed to study the effect of isomeric attachment of keto-ether polyimides on properties such as glass transition temperature and solubility. However, little work has been reported on the relation of polyimide structure to mechanical properties. The purpose of this study was to determine the effect of structural changes in the backbone of keto-ether polyimides on their mechanical properties, specifically, unoriented thin film tensile properties. This study was conducted in two stages. The purpose of the initial stage was to examine the physical and mechanical properties of a representative group (four) of polyimide systems to determine the optimum solvent and cure cycle requirements. These optimum conditions were then utilized in the second stage to prepare films of keto-ether polyimides which were evaluated for mechanical and physical properties. All of the polyimides were prepared using isomers of oxydianiline (ODA) and diaminobenzophenone (DABP) in combination with 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA) and 4,4'-oxydiphthalic anhydride (ODPA).

Mechanical properties of HDPE/UHMWPE blends: effect of filler loading and filler treatment.

PubMed

Lai, K L K; Roziyanna, A; Ogunniyi, D S; Zainal, Arifin M I; Azlan, Ariffin A

2004-05-01

Various blend ratios of high-density polyethylene (HDPE) and ultra high molecular weight polyethylene (UHMWPE) were prepared with the objective of determining their suitability as biomaterials. In the unfilled state, a blend of 50/50 (HDPE/UHMWPE) ratio by weight was found to yield optimum properties in terms of processability and mechanical properties. Hydroxyapatite (HA) was compounded with the optimum blend ratio. The effects of HA loading, varied from 0 to 50wt% for both filled and unfilled blends were tested for mechanical properties. It was found that the inclusion of HA in the blend led to a remarkable improvement of mechanical properties compared to the unfilled blend. In order to improve the bonding between the polymer blend and the filler, the HA used was chemically treated with a coupling agent known as 3-(trimethoxysiyl) propyl methacrylate and the treated HA was mixed into the blend. The effect of mixing the blend with silane-treated HA also led to an overall improvement of mechanical properties.

Process Optimization of Bismaleimide (BMI) Resin Infused Carbon Fiber Composite

NASA Technical Reports Server (NTRS)

Ehrlich, Joshua W.; Tate, LaNetra C.; Cox, Sarah B.; Taylor, Brian J.; Wright, M. Clara; Caraccio, Anne J.; Sampson, Jeffery W.

2013-01-01

Bismaleimide (BMI) resins are an attractive new addition to world-wide composite applications. This type of thermosetting polyimide provides several unique characteristics such as excellent physical property retention at elevated temperatures and in wet environments, constant electrical properties over a vast array of temperature settings, and nonflammability properties as well. This makes BMI a popular choice in advance composites and electronics applications [I]. Bismaleimide-2 (BMI-2) resin was used to infuse intermediate modulus 7 (IM7) based carbon fiber. Two panel configurations consisting of 4 plies with [+45deg, 90deg]2 and [0deg]4 orientations were fabricated. For tensile testing, a [90deg]4 configuration was tested by rotating the [0deg]4 configirration to lie orthogonal with the load direction of the test fixture. Curing of the BMI-2/IM7 system utilized an optimal infusion process which focused on the integration of the manufacturer-recommended ramp rates,. hold times, and cure temperatures. Completion of the cure cycle for the BMI-2/IM7 composite yielded a product with multiple surface voids determined through visual and metallographic observation. Although the curing cycle was the same for the three panellayups, the surface voids that remained within the material post-cure were different in abundance, shape, and size. For tensile testing, the [0deg]4 layup had a 19.9% and 21.7% greater average tensile strain performance compared to the [90deg]4 and [+45deg, 90deg, 90deg,-45degg] layups, respectively, at failure. For tensile stress performance, the [0deg]4 layup had a 5.8% and 34.0% greater average performance% than the [90deg]4 and [+45deg, 90deg, 90deg,-45deg] layups.

Property evolution during vitrification of dimethacrylate photopolymer networks.

PubMed

Abu-elenain, Dalia A; Lewis, Steven H; Stansbury, Jeffrey W

2013-11-01

This study seeks to correlate the interrelated properties of conversion, shrinkage, modulus and stress as dimethacrylate networks transition from rubbery to glassy states during photopolymerization. An unfilled BisGMA/TEGDMA resin was photocured for various irradiation intervals (7-600 s) to provide controlled levels of immediate conversion, which was monitored continuously for 10 min. Fiber optic near-infrared spectroscopy permitted coupling of real-time conversion measurement with dynamic polymerization shrinkage (linometer), modulus (dynamic mechanical analyzer) and stress (tensometer) development profiles. The varied irradiation conditions produced final conversion ranging from 6% to more than 60%. Post-irradiation conversion (dark cure) was quite limited when photopolymerization was interrupted either at very low or very high levels of conversion while significant dark cure contributions were possible for photocuring reactions suspended within the post-gel, rubbery regime. Analysis of conversion-based property evolution during and subsequent to photocuring demonstrated that the shrinkage rate increased significantly at about 40% conversion followed by late-stage suppression in the conversion-dependent shrinkage rate that begins at about 45-50% conversion. The gradual vitrification process over this conversion range is evident based on the broad but well-defined inflection in the modulus versus conversion data. As limiting conversion is approached, modulus and, to a somewhat lesser extent, stress rise precipitously as a result of vitrification with the stress profile showing little if any late-stage suppression as seen with shrinkage. Near the limiting conversion for this model resin, the volumetric polymerization shrinkage rate slows while an exponential rise in modulus promotes the vitrification process that appears to largely dictate stress development. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Polymer, metal and ceramic matrix composites for advanced aircraft engine applications

NASA Technical Reports Server (NTRS)

Mcdanels, D. L.; Serafini, T. T.; Dicarlo, J. A.

1985-01-01

Advanced aircraft engine research within NASA Lewis is being focused on propulsion systems for subsonic, supersonic, and hypersonic aircraft. Each of these flight regimes requires different types of engines, but all require advanced materials to meet their goals of performance, thrust-to-weight ratio, and fuel efficiency. The high strength/weight and stiffness/weight properties of resin, metal, and ceramic matrix composites will play an increasingly key role in meeting these performance requirements. At NASA Lewis, research is ongoing to apply graphite/polyimide composites to engine components and to develop polymer matrices with higher operating temperature capabilities. Metal matrix composites, using magnesium, aluminum, titanium, and superalloy matrices, are being developed for application to static and rotating engine components, as well as for space applications, over a broad temperature range. Ceramic matrix composites are also being examined to increase the toughness and reliability of ceramics for application to high-temperature engine structures and components.

Advanced Strain-Isolation-Pad Material with Bonded Fibrous Construction

NASA Technical Reports Server (NTRS)

Seibold, R. W.; Saito, C. A.; Buller, B. W.

1982-01-01

The feasibility of utilizing air lay and liquid lay felt deposition techniques to fabricate strain isolation pad (SIP) materials for the Space Shuttle Orbiter was demonstrated. These materials were developed as candidate replacements for the present needled felt SIP used between the ceramic tiles and the aluminum skin on the undersurface of the Orbiter. The SIP materials that were developed consisted of high temperature aramid fibers deposited by controlled fluid (air or liquid) carriers to form low density unbonded felts. The deposited felts were then bonded at the fiber intersections with a small amount of high temperature polyimide resin. This type of bonded felt construction can potentially eliminate two of the problems associated with the present SIP, viz., transmittal of localized stresses into the tiles and load history dependent mechanical response. However, further work is needed to achieve adequate through thickness tensile strength in the bonded felts.

Design, Fabrication and Test of Multi-Fiber Laminates

NASA Technical Reports Server (NTRS)

Pike, R. A.; Novak, R. C.

1975-01-01

Unidirectional and angleply multifiber laminates were tested for improved impact strength and other mechanical properties. The effects of several variables on the mechanical properties of epoxy matrix materials were described. These include fiber type (HMS and AS graphites, glass, and Kevlar 49), ratio of primary to hybridizing fiber and hybrid configuration. It is demonstrated that AS graphite/S glass in an intraply configuration results in the best combination of static and Charpy impact properties as well as superior ballistic impact resistance. Pendulum impact tests which were conducted on thin specimens are shown to produce different ranking of materials than tests conducted on standard thickness Charpy specimens. It is shown that the thin specimen results are in better agreement with the ballistic impact data. Additional static test data are reported as a function of temperature for the seven best hybrid configurations having epoxy, polyimide (PMR-15) and polyphenylquinoxaline resins as the matrix.

Aerospace applications of PMR polyimide composites

NASA Technical Reports Server (NTRS)

Serafini, T. T.

1985-01-01

The current status of the novel class of processable, addition-type polyimides known as PMR (for in situ polymerization of monomer reactants) polyimides, developed by NASA at the Lewis Research Center, is reviewed. Highlights of PMR technology studies conducted at NASA Lewis are presented. Several examples of industrial applications of PMR-15 polyimide composites to aerospace structural components are examined.

Substituted Cyclohexene Endcaps for Polymers with Thermal-Oxidative Stability

NASA Technical Reports Server (NTRS)

2005-01-01

This invention relates to polyimides having improved thermal-oxidative stability, to the process of preparing said polyimides, and the use of polyimide prepolymers in the preparation of prepregs and composites. The polyimides are particularly usefull in the preparation of fiber-reinforced, high-temperature composites for use in various engine parts including inlets, fan ducts, exit flaps and other parts of high speed aircraft. The polyimides are derived from the polymerization of effective amounts of at least one tetracarboxylic dianhydride, at least one polyamine and a novel dicarboxylic endcap having the formula presented.

Flexible Microstrip Circuits for Superconducting Electronics

NASA Technical Reports Server (NTRS)

Chervenak, James; Mateo, Jennette

2013-01-01

Flexible circuits with superconducting wiring atop polyimide thin films are being studied to connect large numbers of wires between stages in cryogenic apparatus with low heat load. The feasibility of a full microstrip process, consisting of two layers of superconducting material separated by a thin dielectric layer on 5 mil (approximately 0.13 mm) Kapton sheets, where manageable residual stress remains in the polyimide film after processing, has been demonstrated. The goal is a 2-mil (approximately 0.051-mm) process using spin-on polyimide to take advantage of the smoother polyimide surface for achieving highquality metal films. Integration of microstrip wiring with this polyimide film may require high-temperature bakes to relax the stress in the polyimide film between metallization steps.

Status review of PMR polyimides

NASA Technical Reports Server (NTRS)

Serafini, T. T.

1978-01-01

The current status of first and second generation PMR polyimides are reviewed. Synthesis, processing, and applications were considered, using prepreg materials based on processable, high temperature resistant polyimides.

The AFIT Multielectrode Array for Neural Recording and Simulation: Design, Testing, and Encapsulation

DTIC Science & Technology

1993-12-01

the Device ........................ 13 2.3.1 Silicon Nitride Passivation ................. 13 2.3.2 Polyimide Passivation ................... 14 2.4...Coating .......... ... 49 5.4 Applying the Polyimide ........................ 50 5.4.1 Application of the Polyimide ............ ... 52 5.4.2 Negative...Photo-resist Process ............... 52 5.4.3 Polyimide Etch ........................ 53 5.4.4 Final Cure ............................ 54 5.4.5

Modified Single-Wall Carbon Nanotubes for Reinforce Thermoplastic Polyimide

NASA Technical Reports Server (NTRS)

Lebron-COlon, Marisabel; Meador, Michael A.

2006-01-01

A significant improvement in the mechanical properties of the thermoplastic polyimide film was obtained by the addition of noncovalently functionalized single-wall carbon nanotubes (SWNTs). Polyimide films were reinforced using pristine SWNTs and functionalized SWNTs (F-SWNTs). The tensile strengths of the polyimide films containing F-SWNTs were found to be approximately 1.4 times higher than those prepared from pristine SWNTs.

Fundamental Insight on Developing Low Dielectric Constant Polyimides

NASA Technical Reports Server (NTRS)

Simpson, J. O.; SaintClair, A. K.

1997-01-01

Thermally stable, durable, insulative polyimides are in great demand for the fabrication of microelectronic devices. In this investigation dielectric and optical properties have been studied for several series of aromatic polyimides. The effect of polarizability, fluorine content, and free volume on dielectric constant was examined. In general, minimizing polarizability, maximizing free volume and fluorination all lowered dielectric constants in the polyimides studied.

Helping Aircraft Engines Lighten Up

NASA Technical Reports Server (NTRS)

2004-01-01

High-temperature polyimide/carbon fiber matrix composites are developed by the Polymers Branch at NASA's Glenn Research Center. These materials can withstand high temperatures and have good processing properties, which make them particularly useful for jet and rocket engines and for components such as fan blades, bushings, and duct segments. Applying polyimide composites as components for aerospace structures can lead to substantial vehicle weight reductions. A typical polyimide composite is made up of layers of carbon or glass fibers glued together by a high-temperature polymer to make the material strong, stiff, and lightweight. Organic molecules containing carbon, nitrogen, oxygen, and hydrogen within the polyimide keep the material s density low, resulting in the light weight. The strength of a component or part made from a polyimide comes mainly from the reinforcing high-strength fibers. The strength of the carbon fibers coupled with the stiffness of polyimides allows engineers to make a very rigid structure without it being massive. Another benefit of a polyimide s suitability for aerospace applications is its reduced need for machining. When polyimide parts are removed from a mold, they are nearly in their final shape. Usually, very little machining is needed before a part is ready for use.

Effect of protective coating on microhardness of a new glass ionomer cement: Nanofilled coating versus unfilled resin.

PubMed

Faraji, Foad; Heshmat, Haleh; Banava, Sepideh

2017-01-01

EQUIA TM is a new gastrointestinal (GI) system with high compressive strength, surface microhardness (MH), and fluoride release potential. This in vitro study aimed to assess the effect of aging and type of protective coating on the MH of EQUIA TM GI cement. A total of 30 disc-shaped specimens measuring 9 mm in diameter and 2 mm in thickness were fabricated of EQUIA TM GI and divided into three groups of G-Coat nanofilled coating (a), no coating (b) and margin bond (c). The Vickers MH value of specimens was measured before (baseline) and at 3 and 6 months after water storage. Data were analyzed using repeated measures ANOVA. Group B had significantly higher MH than the other two groups at baseline. Both G-Coat and margin bond increased the surface MH of GI at 3 and 6 months. The MH values of G-Coat and margin bond groups did not significantly increase or decrease between 3 and 6 months. The increase in MH was greater in the G-Coat compared to the margin bond group in the long-term. Clinically, margin bond may be a suitable alternative when G-Coat is not available.

Aromatic Polyimide Foam

NASA Technical Reports Server (NTRS)

Weiser, Erik S. (Inventor); St.Clair, Terry L. (Inventor); Echigo, Yoshiaki (Inventor); Kaneshiro, Hisayasu (Inventor)

2000-01-01

A mechanically undensified aromatic polyimide foam is made from an aromatic polyimide precursor solid residuum and has the following combination of properties: a density according to ASTM D-3574A of about 0.5 pounds/cu.ft to about 20 pounds/cu.ft; a compression strength according to ASTM D-3574C of about 1.5 psi to about 1500 psi; and a limiting oxygen index according to ASTM D-2863 of about 35% oxygen to about 75% oxygen at atmospheric pressure. The aromatic polyimide foam has no appreciable solid inorganic contaminants which are residues of inorganic blowing agents. The aromatic polyimide which constitutes the aromatic polyimide foam has a glass transition temperature (Tg) by differential scanning calorimetry of about 235 C to about 400 C; and a thermal stability of 0 to about 1% weight loss at 204 C as determined by thermogravinietric analysis (TGA). The aromatic polyimide foam has utility as foam insulation and as structural foam, for example, for aeronautical, aerospace and maritime applications.

Polyimides based on 4,4'-bis (4-aminophenoxy)-2,2'or 2,2', 6,6'-substituted biphenyl

NASA Technical Reports Server (NTRS)

Chuang, Chun-Hua K. (Inventor)

1999-01-01

This invention relates the novel diamines, the polyimide oligomers and the polyimides derived therefrom and to the method of preparing the diamines, oligomers and the polyimides. The thermoplastic polyimides derived from the aromatic diamines of this invention are characterized as having a high glass transition temperature, good mechanical properties and improved processability in the manufacture of adhesives, electronic and composite materials for use in the automotive and aerospace industry. The distinction of the novel aromatic diamines of this invention is the 2,2',6,6'-substituted biphenyl radicals which exhibit noncoplanar conformation that enhances the solubility of the diamine as well as the processability of the polyimides, while retaining a realatively high glass transition temperature and improved mechanical properties at useful temperature ranges.

Aromatic Diamines and Polyimides Based on 4,4'-Bis-(4-Aminophenoxy)-2,2' or 2,2',6,6'- Substituted Biphenyl

NASA Technical Reports Server (NTRS)

Chuang, Chun-Hua K. (Inventor)

2000-01-01

This invention relates the novel diamines. the polyimide oligomers and the polyimides derived therefrom and to the method of preparing the diamines, oligomers and the polyimides. The thermoplastic polyimides derived from the aromatic diamines of this invention are characterized as having a high glass transition temperature. good mechanical properties and improved processability in the manufacture of adhesives. electronic and composite materials for use in the automotive and aerospace industry. The distinction of the novel aromatic diamines of this invention is the 2.2',6.6substituted biphenyl radicals which exhibit noncoplanar conformation that enhances the solubility of the diamine as well as the processability of the polyimides. while retaining a relatively high glass transition temperature and improved mechanical properties at useful temperature ranges.

Exploration of photosensitive polyimide as the modification layer in thin film microcircuit

NASA Astrophysics Data System (ADS)

Liu, Lily; Song, Changbin; Xue, Bin; Li, Jing; Wang, Junxi; Li, Jinmin

2018-02-01

Positive type photosensitive polyimide is used as the modification layer in the thin film transistors production process. The photosensitive polyimide is not only used as the second insulating layer, it can also be used instead of a mask because of the photosensitivity. A suitable curing condition can help photosensitive polyimide form the high performance polyimide with orderly texture inside, and the performance of imidization depends on the precise control of temperature, time, and heat control during the curing process. Therefore, experiments of different stepped up heating tests are made, and the ability of protecting silicon dioxide is analyzed.

Polyimide amic acid salts and polyimide membranes formed therefrom

DOEpatents

Ding, Yong; Bikson, Benjamin; Nelson, Joyce Katz; Macheras, James Timothy

2004-04-06

The invention relates to preparation and uses of novel polymeric materials, polyimide amic acid salts (PIAAS). The use of these materials for the fabrication of fluid separation membranes is further disclosed.

Improvements to the Synthesis of Polyimide Aerogels

NASA Technical Reports Server (NTRS)

Meador, Mary Ann B.; Nguyen, Baochau N.; Guo, Haiquan; Vivod, Stephanie; He, Zuhui; Malow, Ericka; Silva, Rebecca

2011-01-01

Cross-linked polyimide aerogels are viable approach to higher temperature, flexible insulation for inflatable decelerators. Results indicate that the all-polyimide aerogels are as strong or stronger than polymer reinforced silica aerogels at the same density. Currently, examining use of carbon nanofiber and clay nanoparticles to improve performance. Flexible, polyimide aerogels have potential utility in other applications such as space suits, habitats, shelter applications, etc. where low dusting is desired

Development of graphite/polyimide honeycomb core materials

NASA Technical Reports Server (NTRS)

Stone, R. H.

1978-01-01

Honeycomb panel constructions consisting entirely of graphite/polyimide composites were developed and evaluated. Graphite/polyimide composites, were used in the honeycomb core webs and in pre-cured sandwich skins. Polyimide adhesives were also developed and evaluated for use in skin-core bonding. The purpose of this program was to develop light weight sandwich constructions for high temperature applications which could provide comparable shear strength and stiffness to metallic honeycomb constructions.

PMR polyimides-review and update

NASA Technical Reports Server (NTRS)

Serafini, T. T.; Delvigs, P.; Alston, W. B.

1982-01-01

Fiber reinforced PMR polyimides are finding increased acceptance as engineering materials for high performance structural applications. Prepreg materials based on this novel class of highly processable, high temperature resistant polyimides are commercially available and the PMR concept is used by other investigators. The current status of first and second generation PMR polyimides were reviewed. Emphasis is given to the chemistry, processing and applications of the first generation material known as PMR-15.

The effect of elastomer chain length on properties of silicone-modified polyimide adhesives

NASA Technical Reports Server (NTRS)

St.clair, A. K.; St.clair, T. L.; Ezzell, S.

1981-01-01

A series of polyimides containing silicone elastomers was synthesized in order to study the effects of the elastomer chain length on polymer properties. The elastomer with repeat units varying from n=10 to 105 was chemically reacted into the backbone of an addition polyimide oligomer via reactive aromatic amine groups. Glass transition temperatures of the elastomer and polyimide phases were observed by torsional braid analysis. The elastomer-modified polyimides were tested as adhesives for bonding titanium in order to determine their potential for aerospace applications. Adhesive lap shear tests were performed before and after aging bonded specimens at elevated temperatures.

Polyimides containing carbonyl and ether connecting groups - II

NASA Technical Reports Server (NTRS)

Hergenrother, P. M.; Havens, S. J.

1989-01-01

In a study of polyimides containing carbonyl and ether connecting groups between aromatic rings, several new polyimides were prepared and characterized. A few of these polymers were semicrystalline. Glass transition temperatures ranged from 164 to 258 C, and crystalline melt temperatures were observed between 350 and 424 C. The semicrystalline polyimide from the reaction of 3.3',4,4'-benzophenonetetracarboxylic dianhydride and 1,3-bis(4-aminophenoxy-4'-benzoyl)benzene provided transparent orange films with excellent tensile properties, exceptional resistance to solvents and strong base, and high thermooxidative stability. In addition, this polyimide provided excellent adhesive strength for joining titanium (6Al-4V) to titanium.

Effect of Temperature and Deformation Rate on the Tensile Mechanical Properties of Polyimide Films

NASA Technical Reports Server (NTRS)

Moghazy, Samir F.; McNair, Kevin C.

1996-01-01

In order to study the structure-property relationships of different processed oriented polyimide films, the mechanical properties will be identified by using tensile tester Instron 4505 and structural information such as the 3-dimensional birefringence molecular symmetry axis and 3-dimensional refractive indices will be determined by using wave guide coupling techniques. The monoaxial drawing techniques utilized in this research are very useful for improving the tensile mechanical properties of aromatic polyimide films. In order to obtain high modulus/high strength polyimide films the following two techniques have been employed, cold drawing in which polyimide films are drawn at room temperature at different cross head speeds and hot drawing in which polyimide films are drawn at different temperatures and cross head speeds. In the hot drawing process the polyimide films are drawn at different temperatures until the glass transition temperature (Tg) is reached by using the environmental chamber. All of the mechanical and optical property parameters will be identified for each sample processed by both cold and hot drawing techniques.

Incorporation of metal ions into polyimides

NASA Technical Reports Server (NTRS)

Taylor, L. T.; Carver, V. C.; Furtsch, T. A.; Saint Clair, A. K.

1980-01-01

The effects of the incorporation of metal ions into various polyimides on polyimide properties are investigated. Polyimide films derived from 3,3',4,4'-benzophenone tetracarboxylic acid dianhydride (BDTA) 3,3'-diaminobenzophenone (m,m'-DABP), 4,4'-diaminobenzophenone (p,p'-DABP) or 4,4'-oxydianiline were prepared with the concurrent addition of approximately 20 metals in a variety of forms. In general, it is found that the films derived from BDTA + p,p'-DABP were brittle and of poor quality, with brittle films also produced in most of the BDTA + m, m'-DABP polyimides regardless of whether the added metal was hydrate or anhydrous. Thermomechanical analysis, torsional braid analysis, thermal gravimetric analysis, infrared spectral analysis and isothermal studies on many of the polyimide films produced indicate that the softening temperature is generally increased upon the addition of metal ions, at the expense of thermal stability, while no changes in chemical functionality are observed. The best system studied in regard to polymer property enhancement appears to be tri(acetylacetonato)aluminum(III) added to the m, m'-DABP polyamide, which has been found to exhibit four times the lap shear strength of the polyimide alone.

Design and Fabrication of an Implantable Cortical Semiconductor Integrated Circuit Electrode Array

DTIC Science & Technology

1990-12-01

25 Array Pads....................25 Polyimide ....................26 III. METHODOLOGY.........................27 Brain Chip Electronics...38 Ionic Permeation. .................. 38 Polyimide . ................... 38 Implantation. .................... 39 Wire Bonding...53 Pad Sensitivity ................. 53 Ionic Permeat:.on. .................. 54 Polyimide . ................... 54 Implantation

Advanced Design Composite Aircraft

DTIC Science & Technology

1976-02-01

been selected for ADCA applications. These are graphite (PAN)/ epoxy, graphite (PAN)/polyimide, Kevlar /epoxy, f ibergl ass/epoxy, and quartz...Aluminum Alloy Aluminum Alloy ACG (commercial grade) Nomex HRP Fiberglass/ Phenolic HRH Fiberglass/Polyimide Graphite/epoxy Graphi te/Polyimide

Polyimide foams provide thermal insulation and fire protection

NASA Technical Reports Server (NTRS)

Rosser, R. W.

1972-01-01

Chemical reactions to produce polyimide foams for application as thermal insulation and fire prevention materials are discussed. Thermal and physical properties of the polyimides are described. Methods for improving basic formulations to produce desired qualitites are included.

High-temperature polyimides prepared from 2,2-bis-[(2-halo-4-aminophenoxy)-phenyl]hexafluoropropane

NASA Technical Reports Server (NTRS)

Jones, Robert J. (Inventor); Chang, Glenn E. C. (Inventor)

1984-01-01

There are provided the aromatic diamines 2,2-bis-[(2-halo-4-aminophenoxy)-phenyl]hexafluoropropane, where the attached ortho halogen is preferably chlorine, and 4,4'-bis(4-aminophenoxy)biphenyl, as novel monomers for polyimide polymerizations. The former, when reacted with 2,2-bis(3,4-dicarboxyphenyl)hexafluoropropane dianhydride, provides a polyimide having exceptional high-temperature performance. The latter diamine is a low-cost monomer for polyimide production.

Surface interaction of polyimide with oxygen ECR plasma

NASA Astrophysics Data System (ADS)

Naddaf, M.; Balasubramanian, C.; Alegaonkar, P. S.; Bhoraskar, V. N.; Mandle, A. B.; Ganeshan, V.; Bhoraskar, S. V.

2004-07-01

Polyimide (Kapton-H), was subjected to atomic oxygen from an electron cyclotron resonance plasma. An optical emission spectrometer was used to characterize the atomic oxygen produced in the reactor chamber. The energy of the ions was measured using a retarding field analyzer, placed near the substrate. The density of atomic oxygen in the plasma was estimated using a nickel catalytic probe. The surface wettability of the polyimide samples monitored by contact angle measurements showed considerable improvement when treated with plasma. X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopic studies showed that the atomic oxygen in the plasma is the main specie affecting the surface chemistry and adhesion properties of polyimide. The improvement in the surface wettability is attributed to the high degree of cross-linking and large concentration of polar groups generated in the surface region of polyimide, after plasma treatment. The changes in the surface region of polyimide were observed by atomic force microscopic analysis.

Surface Evaluation by X-Ray Photoelectron Spectroscopy of High Performance Polyimide Foams After Exposure to Oxygen Plasma

NASA Technical Reports Server (NTRS)

Melendez, Orlando; Hampton, Michael D.; Williams, Martha K.; Brown, Sylvia F.; Nelson, Gordon L.; Weiser, Erik S.

2002-01-01

Aromatic polyimides have been attractive in the aerospace and electronics industries for applications such as cryogenic insulation, flame retardant panels and structural subcomponents. Newer to the arena of polyimides is the synthesis of polyimide foams and their applications. In the present work, three different, closely related, polyimide foams developed by NASA Langley Research Center (LaRC) are studied by X-ray Photoelectron Spectroscopy (XPS) after exposure to radio frequency generated Oxygen Plasma. Although polyimide films exposure to atomic oxygen and plasma have been studied previously and reported, the data relate to films and not foams. Foams have much more surface area and thus present new information to be explored. Understanding degradation mechanisms and properties versus structure, foam versus solid is of interest and fundamental to the application and protection of foams exposed to atomic oxygen in Low Earth Orbit (LEO).

Polyimides prepared from 3,5-diamino benzo trifluoride

NASA Technical Reports Server (NTRS)

Gerber, Margaret K. (Inventor); Pratt, J. Richard (Inventor); St.clair, Terry L. (Inventor); St.clair, Anne K. (Inventor)

1993-01-01

High performance, thermooxidatively stable polyimides are prepared by reacting aromatic diamines with pendant trifluoromethyl groups and dianhydrides in an amide solvent to form a poly(amic acid), followed by cyclizing the poly(amic acid) to form the corresponding polyimide.

Low dielectric polyimide aerogels as substrates for lightweight patch antennas.

PubMed

Meador, Mary Ann B; Wright, Sarah; Sandberg, Anna; Nguyen, Baochau N; Van Keuls, Frederick W; Mueller, Carl H; Rodríguez-Solís, Rafael; Miranda, Félix A

2012-11-01

The dielectric properties and loss tangents of low-density polyimide aerogels have been characterized at various frequencies. Relative dielectric constants as low as 1.16 were measured for polyimide aerogels made from 2,2'-dimethylbenzidine (DMBZ) and biphenyl 3,3',4,4'-tetracarbozylic dianhydride (BPDA) cross-linked with 1,3,5-triaminophenoxybenzene (TAB). This formulation was used as the substrate to fabricate and test prototype microstrip patch antennas and benchmark against state of practice commercial antenna substrates. The polyimide aerogel antennas exhibited broader bandwidth, higher gain, and lower mass than the antennas made using commercial substrates. These are very encouraging results, which support the potential advantages of the polyimide aerogel-based antennas for aerospace applications.

Low-Dielectric Constant Polyimide Nanoporous Films: Synthesis and Properties

NASA Astrophysics Data System (ADS)

Mehdipour-Ataei, S.; Rahimi, A.; Saidi, S.

2007-08-01

Synthesis of high temperature polyimide foams with pore sizes in the nanometer range was developed. Foams were prepared by casting graft copolymers comprising a thermally stable block as the matrix and a thermally labile material as the dispersed phase. Polyimides derived from pyromellitic dianhydride with new diamines (4BAP and BAN) were used as the matrix material and functionalized poly(propylene glycol) oligomers were used as a thermally labile constituent. Upon thermal treatment the labile blocks were subsequently removed leaving pores with the size and shape of the original copolymer morphology. The polyimides and foamed polyimides were characterized by some conventional methods including FTIR, H-NMR, DSC, TGA, SEM, TEM, and dielectric constant.

Polyimides with carbonyl and ether connecting groups between the aromatic rings

NASA Technical Reports Server (NTRS)

Hergenrother, Paul M. (Inventor); Havens, Stephen J. (Inventor)

1992-01-01

New polyimides have been prepared from the reaction of aromatic dianhydrides with novel aromatic diamines containing carbonyl and ether connecting groups between the aromatic rings. Several of these polyimides are shown to be semi-crystalline as evidenced by wide angle x ray diffraction and differential scanning calorimetry. Most of the polyimides form tough solvent resistant films with high tensile properties. Several of these materials can be thermally processed to form solvent and base resistant moldings.

Effect of MeV electron irradiation on the free volume of polyimide

NASA Astrophysics Data System (ADS)

Alegaonkar, P. S.; Bhoraskar, V. N.

2004-08-01

The free volume of the microvoids in the polyimide samples, irradiated with 6 MeV electrons, was measured by the positron annihilation technique. The free volume initially decreased the virgin value from similar to13.70 to similar to10.98 Angstrom(3) and then increased to similar to18.11 Angstrom(3) with increasing the electron fluence, over the range of 5 x 10(14) - 5 x 10(15) e/cm(2). The evolution of gaseous species from the polyimide during electron irradiation was confirmed by the residual gas analysis technique. The polyimide samples irradiated with 6 MeV electrons in AgNO3 solution were studied with the Rutherford back scattering technique. The diffusion of silver in these polyimide samples was observed for fluences >2 x 10(15) e/cm(2), at which microvoids of size greater than or equal to3 Angstrom are produced. Silver atoms did not diffuse in the polyimide samples, which were first irradiated with electrons and then immersed in AgNO3 solution. These results indicate that during electron irradiation, the microvoids with size greater than or equal to3 Angstrom were retained in the surface region through which silver atoms of size similar to2.88 Angstrom could diffuse into the polyimide. The average depth of diffusion of silver atoms in the polyimide was similar to2.5 mum.

Processing and Characterization of Graphene/Polyimide-Nickel Oxide Hybrid Nanocomposites for Advanced Energy Storage in Supercapacitor Applications

NASA Astrophysics Data System (ADS)

Okafor, Patricia A.

This research is focused on enhancing electrochemical properties/energy storage capabilities of graphene-polyimide composites. The composite's dense morphology/structure limits ionic penetration owing to high bulk resistances resulting in poor electrochemical performance. Modification of the composite's morphology by incorporation of facile pores during curing increases total available surface area to electrolyte species. Presence of pores increases adsorption sites for double layer formation and increases overall capacitance. In this work, aromatic polyimide precursors were reacted in the presence of nano-graphene fillers to synthesize graphene-polyimide composite films. The resulting composite was very stiff and dense with a high glass transition temperature (Tg) of 400 °C and storage modulus of 7.20 GPa. Selective decomposition of a thermally labile poly(acrylic ester) resin introduced into the composite during synthesis creates pores of varying size and shapes which increases available surface area of embedded stacked graphene sheets available for ion adsorption and double layer formation. Proper control over pore size and specific surface area of pores was required to ensure good performance in terms of both power delivery rate and energy storage capacity. Dynamic mechanical studies on modified composite showed very good mechanical property while shifts in imide peaks to lower wave numbers in Raman and Fourier transform spectroscopy (FTIR) confirms presence of chemical interaction between graphene filler and polymer matrix confirming uniform dispersion of fillers in the material. Thermogravimetric analysis (TGA) shows thermal stability for the composite systems at temperatures above 700°C. To further optimize material's energy storage capabilities, a hybrid composite was formed by depositing relatively cheap nickel oxide onto the modified porous composite system by a two-step process. A remarkable improvement in electrochemical properties up to an order of magnitude was observed. Electrochemical performance of the hybrid system showed strong dependence on deposition current density, deposition time and substrate pore morphology. Increased NiO particle size (aggregates) was observed with increased deposition time and current density which had a significant impact on charge transfer resistance and specific capacitance. Several correlations were made between composite's morphology and obtained properties. The material's morphology showed direct correlation with double layer capacitance, charge capacity, bulk resistance and sheet conductivity measured using cyclic voltammetry (CV), cyclic charge discharge (CCD), electrochemical impedance spectroscopy (EIS) and four probe measurements respectively. It was observed that smaller well distributed pores showed enhanced properties compared to larger pores. Material's overall performance shows a linear dependence on porosity. The overall electrochemical and electrical behavior of the system is directly linked to the composite's morphology and structure as will be demonstrated in this thesis work.

The compressive behaviour and constitutive equation of polyimide foam in wide strain rate and temperature

NASA Astrophysics Data System (ADS)

Yoshimoto, Akifumi; Kobayashi, Hidetoshi; Horikawa, Keitaro; Tanigaki, Kenichi

2015-09-01

These days, polymer foams, such as polyurethane foam and polystyrene foam, are used in various situations as a thermal insulator or shock absorber. In general, however, their strength is insufficient in high temperature environments because of their low glass transition temperature. Polyimide is a polymer which has a higher glass transition temperature and high strength. Its mechanical properties do not vary greatly, even in low temperature environments. Therefore, polyimide foam is expected to be used in the aerospace industry. Thus, the constitutive equation of polyimide foam that can be applied across a wide range of strain rates and ambient temperature is very useful. In this study, a series of compression tests at various strain rates, from 10-3 to 103 s-1 were carried out in order to examine the effect of strain rate on the compressive properties of polyimide foam. The flow stress of polyimide foam increased rapidly at dynamic strain rates. The effect of ambient temperature on the properties of polyimide foam was also investigated at temperature from - 190 °C to 270°∘C. The flow stress decreased with increasing temperature.

Summary Report of the Summer Conference DARPA-Materials Research Council Held in La Jolla, California on 10 July thru 4 August 1989

DTIC Science & Technology

1989-08-04

ceramic substrate and a multilayer thin film metal (copper) and polymer ( polyimide ) overlays. 73 The MCM technology was pioneered by IBM, which has made...packaging. The first is the use of polymeric dielectric layers such as polyimides . In fact, the current MCP’s 3 being developed for the DoD use... polyimide dielectrics. Nonetheless, much work remains to be done before these organic dielectrics can be regarded as Isatisfactory. Polyimides have a

Method of Forming a Hot Film Sensor System on a Model

NASA Technical Reports Server (NTRS)

Tran, Sang Q. (Inventor)

1998-01-01

A method of forming a hot film sensor directly on a model is provided. A polyimide solution is sprayed onto the model. The model so sprayed is then heated in air. The steps of spraying and heating are repeated until a polyimide film of desired thickness is achieved on the model. The model with the polyimide film thereon is then thoroughly dried in air. One or more hot film sensors and corresponding electrical conducting leads are then applied directly onto the polyimide film.

Polyimide processing additives

NASA Technical Reports Server (NTRS)

Fletcher, James C. (Inventor); Pratt, J. Richard (Inventor); St.clair, Terry L. (Inventor); Stoakley, Diane M. (Inventor); Burks, Harold D. (Inventor)

1992-01-01

A process for preparing polyimides having enhanced melt flow properties is described. The process consists of heating a mixture of a high molecular weight poly-(amic acid) or polyimide with a low molecular weight amic acid or imide additive in the range of 0.05 to 15 percent by weight of additive. The polyimide powders so obtained show improved processability, as evidenced by lower melt viscosity by capillary rheometry. Likewise, films prepared from mixtures of polymers with additives show improved processability with earlier onset of stretching by TMA.

Polyimide processing additives

NASA Technical Reports Server (NTRS)

Pratt, J. Richard (Inventor); St.clair, Terry L. (Inventor); Stoakley, Diane M. (Inventor); Burks, Harold D. (Inventor)

1993-01-01

A process for preparing polyimides having enhanced melt flow properties is described. The process consists of heating a mixture of a high molecular weight poly-(amic acid) or polyimide with a low molecular weight amic acid or imide additive in the range of 0.05 to 15 percent by weight of the additive. The polyimide powders so obtained show improved processability, as evidenced by lower melt viscosity by capillary rheometry. Likewise, films prepared from mixtures of polymers with additives show improved processability with earlier onset of stretching by TMA.

The development of aerospace polyimide adhesives

NASA Technical Reports Server (NTRS)

St.clair, A. K.; St.clair, T. L.

1983-01-01

Few materials are available which can be used as aerospace adhesives at temperatures in the range of 300 C. The Materials Division at NASA-Langley Research Center developed several high temperature polyimide adhesives to fulfill the stringent needs of current aerospace programs. These adhesives are the result of a decade of basic research studies on the structure property relationships of both linear and addition aromatic polyimides. The development of both in house and commercially available polyimides is reviewed with regards to their potential for use as aerospace adhesives.

Polyimide Aerogels with Three-Dimensional Cross-Linked Structure

NASA Technical Reports Server (NTRS)

Panek, John

2010-01-01

Polyimide aerogels with three-dimensional cross-linked structure are made using linear oligomeric segments of polyimide, and linked with one of the following into a 3D structure: trifunctional aliphatic or aromatic amines, latent reactive end caps such as nadic anhydride or phenylethynylphenyl amine, and silica or silsesquioxane cage structures decorated with amine. Drying the gels supercritically maintains the solid structure of the gel, creating a polyimide aerogel with improved mechanical properties over linear polyimide aerogels. Lightweight, low-density structures are desired for acoustic and thermal insulation for aerospace structures, habitats, astronaut equipment, and aeronautic applications. Aerogels are a unique material for providing such properties because of their extremely low density and small pore sizes. However, plain silica aerogels are brittle. Reinforcing the aerogel structure with a polymer (X-Aerogel) provides vast improvements in strength while maintaining low density and pore structure. However, degradation of polymers used in cross-linking tends to limit use temperatures to below 150 C. Organic aerogels made from linear polyimide have been demonstrated, but gels shrink substantially during supercritical fluid extraction and may have lower use temperature due to lower glass transition temperatures. The purpose of this innovation is to raise the glass transition temperature of all organic polyimide aerogel by use of tri-, tetra-, or poly-functional units in the structure to create a 3D covalently bonded network. Such cross-linked polyimides typically have higher glass transition temperatures in excess of 300 400 C. In addition, the reinforcement provided by a 3D network should improve mechanical stability, and prevent shrinkage on supercritical fluid extraction. The use of tri-functional aromatic or aliphatic amine groups in the polyimide backbone will provide such a 3D structure.

Rod-Coil Block Polyimide Copolymers

NASA Technical Reports Server (NTRS)

Meador, Mary Ann B. (Inventor); Kinder, James D. (Inventor)

2005-01-01

This invention is a series of rod-coil block polyimide copolymers that are easy to fabricate into mechanically resilient films with acceptable ionic or protonic conductivity at a variety of temperatures. The copolymers consist of short-rigid polyimide rod segments alternating with polyether coil segments. The rods and coil segments can be linear, branched or mixtures of linear and branched segments. The highly incompatible rods and coil segments phase separate, providing nanoscale channels for ion conduction. The polyimide segments provide dimensional and mechanical stability and can be functionalized in a number of ways to provide specialized functions for a given application. These rod-coil black polyimide copolymers are particularly useful in the preparation of ion conductive membranes for use in the manufacture of fuel cells and lithium based polymer batteries.

Polyimide/metal composite films via in situ decomposition of inorganic additives - Soluble polyimide versus polyimide precursor

NASA Technical Reports Server (NTRS)

Rancourt, J. D.; Porta, G. M.; Moyer, E. S.; Madeleine, D. G.; Taylor, L. T.

1988-01-01

Polyimide-metal oxide (Co3O4 or CuO) composite films have been prepared via in situ thermal decomposition of cobalt (II) chloride or bis(trifluoroacetylacetonato)copper(II). A soluble polyimide (XU-218) and its corresponding prepolymer (polyamide acid) were individually employed as the reaction matrix. The resulting composites exhibited a greater metal oxide concentration at the air interface with polyamide acid as the reaction matrix. The water of imidization that is released during the concurrent polyamide acid cure and additive decomposition is believed to promote metal migration and oxide formation. In contrast, XU-218 doped with either HAuCl4.3H2O or AgNO3 yields surface gold or silver when thermolyzed (300 C).

Substrate Material for Holographic Emulsions Utilizing Fluorinated Polyimide Film

NASA Technical Reports Server (NTRS)

Gierow, Paul A. (Inventor); Clayton, William R. (Inventor); St.Clair, Anne K. (Inventor)

1999-01-01

A new holographic substrate utilizing flexible. optically transparent fluorinated polyimides. Said substrates have 0 extremely low birefringence which results in a high signal to noise ratio in subsequent holograms. Specific examples of said fluorinated polyimides include 6FDA+APB and 6FDA+4BDAF.

Polyimides containing meta-biphenylenedioxy moieties and articles prepared therefrom

NASA Technical Reports Server (NTRS)

St.clair, Terry L. (Inventor); Pratt, Richard (Inventor)

1995-01-01

Two monomers containing meta-biphenylenedioxy moieties were prepared. One monomer, a diamine, is used to prepare polyimide, polyamide, and epoxy polymers. The other monomer, a dianhydride, was used to prepared polyimide polymers. These polymers are used to make films, coatings, and selective membranes.

The mechanical stability of polyimide films at high pH

NASA Technical Reports Server (NTRS)

Croall, Catharine I.; St.clair, Terry L.

1990-01-01

Polyimide insulated electrical wire has been widely used in the aerospace industry in commercial, military, and to a lesser degree, general aviation aircraft since the early 1970s. Wiring failures linked to insulation damage have drawn much attention in the media and concerns have developed regarding the long term stability and safety of polyimide insulated electrical wire. The mechanical durability and chemical stability of polyimide insulated wire are affected by hydrolysis, notch propagation, wet and dry arc tracking, topcoat flaking, and degradation due to high pH fluids. Several polyimides were selected for evaluation for resistance to degradation by various aqueous alkaline solutions. The polyimides under evaluation include commercially available films such as KAPTON (tradename), APICAL (tradename), LARC-TPI, and UPILEX (tradename) R and S, as well as a number of experimental films prepared at NASA-Langley. Material properties investigated include viscosity, solubility, moisture absorption, glass transition temperature, dielectric constant, and mechanical properties before and after exposure to various conditions.

Photogeneration of refractive-index patterns in doped polyimide films.

PubMed

Chakravorty, K K

1993-05-01

A photosensitive benzophenone tetracarboxylic dianhyride-alkylated diamine polyimide formulation has been evaluated for application in an optical interconnection area. The refractive-index patterns in this material were optically recorded by UV-assisted photodoping of sensitizers. The polyimide films were selectively doped with benzoin-type photosensitizers such as benzildimethylketal and benzoin ethyl ether, which cause a decrease in the refractive index. High-dose UV irradiation that causes cross linking of the polyimide chains was also employed for augmenting the refractive-index difference to 0.017 between the doped and undoped regions. Refractive-index variations and lightguiding properties were investigated as a function of doping concentrations and other processing conditions. The author utilized this technique for the fabrication of embedded polyimide channel waveguides. The two photosensitizers have different effects on the waveguiding characteristics of the polyimide films. Losses for benzoin ethyl ether remained low whereas doping with benzildimethylketal caused significant increase in the waveguiding loss at high doping concentrations. Near-field imaging of the output from such waveguides shows good confinement of 815-nm light.

Photogeneration of refractive-index patterns in doped polyimide films

NASA Astrophysics Data System (ADS)

Chakravorty, K. K.

1993-05-01

A photosensitive benzophenone tetracarboxylic dianhyride-alkylated diamine polyimide formulation has been evaluated for application in an optical interconnection area. The refractive-index patterns in this material were optically recorded by UV-assisted photodoping of sensitizers. The polyimide films were selectively doped with benzoin-type photosensitizers such as benzildimethylketal and benzoin ethyl ether, which cause a decrease in the refractive index. High-dose UV irradiation that causes cross linking of the polyimide chains was also employed for augmenting the refractive-index difference to 0.017 between the doped and undoped regions. Refractive-index variations and lightguiding properties were investigated as a function of doping concentrations and other processing conditions. The author utilized this technique for the fabrication of embedded polyimide channel waveguides. The two photosensitizers have different effects on the waveguiding characteristics of the polyimide films. Losses for benzoin ethyl ether remained low whereas doping with benzildimethylketal caused significant increase in the waveguiding loss at high doping concentrations. Near-field imaging of the output from such waveguides shows good confinement of 815-nm light.

EFFECTS OF ONE WEEK TRITIUM EXPOSURE ON EPDM ELASTOMER

DOE Office of Scientific and Technical Information (OSTI.GOV)

Clark, E

This report documents test results for the exposure of four formulations of EPDM (ethylene-propylene diene monomer) elastomer to tritium gas at one atmosphere for approximately one week and characterization of material property changes and changes to the exposure gas during exposure. All EPDM samples were provided by Los Alamos National Laboratory (LANL). Material properties that were characterized include mass, sample dimensions, appearance, flexibility, and dynamic mechanical properties. The glass transition temperature was determined by analysis of the dynamic mechanical property data per ASTM standards. No change of glass transition temperature due to the short tritium gas exposure was observed. Filledmore » and unfilled formulations of Dupont{reg_sign} Nordel{trademark} 1440 had a slightly higher glass transition temperature than filled and unfilled formulations of Uniroyal{reg_sign} Royalene{reg_sign} 580H; filled formulations had the same glass transition as unfilled. The exposed samples appeared the same as before exposure--there was no evidence of discoloration, and no residue on stainless steel spacers contacting the samples during exposure was observed. The exposed samples remained flexible--all formulations passed a break test without failing. The unique properties of polymers make them ideal for certain components in gas handling systems. Specifically, the resiliency of elastomers is ideal for sealing surfaces, for example in valves. EPDM, initially developed in the 1960s, is a hydrocarbon polymer used extensively for sealing applications. EPDM is used for its excellent combination of properties including high/low-temperature resistance, radiation resistance, aging resistance, and good mechanical properties. This report summarizes initial work to characterize effects of tritium gas exposure on samples of four types of EPDM elastomer: graphite filled and unfilled formulations of Nordel{trademark} 1440 and Royalene{reg_sign} 580H.« less

Low dielectric constant and moisture-resistant polyimide aerogels containing trifluoromethyl pendent groups

NASA Astrophysics Data System (ADS)

Wu, Tingting; Dong, Jie; Gan, Feng; Fang, Yuting; Zhao, Xin; Zhang, Qinghua

2018-05-01

Conventional polyimide aerogels made from biphenyl-3,3‧,4,4‧-tetracarboxylic dianydride (BPDA) and 4,4‧-oxidianiline (ODA) exhibit poor resistance to moisture and mechanical properties. In this work, a versatile diamine, 2,2‧-bis-(trifluoromethyl)-4,4‧-diaminobiphenyl (TFMB), is introduced to BPDA/ODA backbone to modify the comprehensive performance of this aerogel. Among all formulations, the resulted polyimide aerogels exhibit the lowest shrinkage and density as well as highest porosity, at the ODA/TFMB molar ratio of 5/5. Dielectric constants and loss tangents of the aerogels fall in the range of 1.29-1.33 and 0.001-0.004, respectively, and more TFMB fractions results in a slightly decrease of dielectric constant and loss tangent. In addition, moisture-resistance of the aerogels are dramatically enhanced as the water absorption decreasing from 415% for BPDA/ODA to 13% for the polyimide aerogel at the ODA/TFMB molar ratio of 7/3, and even to 4% for the homo-BPDA/TFMB polyimide aerogel, showing a superhydrophobic characteristic, which is a great advantage for polyimide aerogels used as low dielectric materials. Meanwhile, all of formulations of aerogels exhibit high absorption capacities for oils and common organic solvents, indicating that these fluorinated polyimide aerogels are good candidates for the separation of oils/organic solvents and water. Mechanical properties and thermal stability of the polyimide aerogels are also raised to varying degrees due to the rigid-rod biphenyl structure introduced by TFMB.

New rapid-curing, stable polyimide polymers with high-temperature strength and thermal stability

NASA Technical Reports Server (NTRS)

Burns, E. A.; Jones, J. F.; Kendrick, W. R.; Lubowitz, H. R.; Thorpe, R. S.; Wilson, E. R.

1969-01-01

Additive-type polymerization reaction forms thermally stable polyimide polymers, thereby eliminating the volatile matter attendant with the condensation reaction. It is based on the utilization of reactive alicyclic rings positioned on the ends of polyimide prepolymers having relatively low molecular weights.

Synthesis and Characterization of Polyimides with Ether Linkages

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.; Fu, Joyce; Scheiman, Daniel A.

1998-01-01

A series of polyimides derived from a newly synthesized diamine, namely, 4,4-bis(4-aminophenoxy)-2,2-dimethylbiphenyl (BAPD), were developed and characterized. Their physical and thermal properties were compared to polyimides based on'commercially available 2,2-bis(4-(4-aminophenoxy)phenyl)propane (BAPP).

High density circuit technology, part 2

NASA Technical Reports Server (NTRS)

Wade, T. E.

1982-01-01

A multilevel metal interconnection system for very large scale integration (VLSI) systems utilizing polyimides as the interlayer dielectric material is described. A complete characterization of polyimide materials is given as well as experimental methods accomplished using a double level metal test pattern. A low temperature, double exposure polyimide patterning procedure is also presented.

77 FR 62259 - Certain Polyimide Films, Products Containing Same, and Related Methods Commission Determination...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-10-12

... INTERNATIONAL TRADE COMMISSION [Investigation No. 337-TA-772] Certain Polyimide Films, Products... polyimide films, products containing same, and related methods by reason of infringement of one or more of... prong of the domestic industry requirement. Id. With respect to the `961 patent, the Commission...

77 FR 47092 - Certain Polyimide Films, Products Containing Same, and Related Methods; Notice of Commission...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-08-07

... INTERNATIONAL TRADE COMMISSION [Investigation No. 337-TA-772] Certain Polyimide Films, Products Containing Same, and Related Methods; Notice of Commission Determination to Partially Review and Partially... polyimide films, products containing same, and related methods by reason of infringement of one or more of...

Diphenylmethane-containing dianhydride and polyimides prepared therefrom

NASA Technical Reports Server (NTRS)

St.clair, Anne K. (Inventor); Boston, Harold G. (Inventor); Pratt, J. Richard (Inventor)

1993-01-01

A high temperature stable, highly optically transparent-to-colorless, low dielectic linear aromatic polyimide is prepared by reacting an aromatic diamine with 3,3'bis (3,4-dicarboxyphenoxy) diphenylmethane dianhydride in an amide solvent to form a linear aromatic polyamic acid. This polyamic acid is then cyclized to form the corresponding polyimide.

Preparing composite materials from matrices of processable aromatic polyimide thermoplastic blends

NASA Technical Reports Server (NTRS)

Johnston, Norman J. (Inventor); St.clair, Terry L. (Inventor); Baucom, Robert M. (Inventor); Gleason, John R. (Inventor)

1991-01-01

Composite materials with matrices of tough, thermoplastic aromatic polyimides are obtained by blending semi-crystalline polyimide powders with polyamic acid solutions to form slurries, which are used in turn to prepare prepregs, the consolidation of which into finished composites is characterized by excellent melt flow during processing.

Status review of PMR polyimides. [Polymerization of Monomer Reactants

NASA Technical Reports Server (NTRS)

Serafini, T. T.

1979-01-01

In the NASA developed PMR (polymerization of monomer reactants) the reinforcing fibers are impregnated with a solution containing a mixture of monomers dissolved in a low boiling point alkyl alcohol solvent, with the monomers reacting in situ at elevated temperatures to form a thermo-oxidatively stable polyimide matrix. The current status of first and second generation PMR polyimides is reviewed, considering synthesis and properties, processing, and applications. It is concluded that the PMR approach offers various significant advantages, especially superior high temperature properties and processing versatility, to fabricators and users of polyimide/fiber composites.

Thermal History Of PMRs Via Pyrolysis-Gas Chromatography

NASA Technical Reports Server (NTRS)

Gluyas, Richard E.; Alston, William B.; Snyder, William J.

1994-01-01

Pyrolysis-gas chromatography (PY-GC) useful as analytical technique to determine extents of cure or postcure of PMR-15 polyimides and to lesser extent, cumulative thermal histories of PMR-15 polyimides exposed to high temperatures. Also applicable for same purposes to other PMR polyimides and to composite materials containing PMR polyimides. Valuable in reducing costs and promoting safety in aircraft industry by helping to identify improperly cured or postcured PMR-15 composite engine and airframe components and helping to identify composite parts nearing ends of their useful lives.

Phenylated polyimides prepared from 3,6-diarylpyromellitic dianhydride and aromatic diamines

NASA Technical Reports Server (NTRS)

Harris, Frank W. (Inventor)

1992-01-01

A new class of soluble phenylated polyimides made from 3,6-diarypyromellitic dianhydride and process for the manufacture of the 3,6-diarypyromellitic dianhydride starting material. The polyimides obtained with said dianhydride are readily soluble in appropriate organic solvents and are distinguished by excellent thermal, electrical and/or mechanical properties making the polyimides ideally suited as coating materials for microelectronic apparatii, as membranes for selective molecular separation or permeation or selective gas separation or permeation, or as reinforcing fibers in molecular composites, or as high modulus, high tensile strength fibers.

Improvement of the relaxation time and the order parameter of nematic liquid crystal using a hybrid alignment mixture of carbon nanotube and polyimide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, Hyojin; Yang, Seungbin; Lee, Ji-Hoon, E-mail: jihoonlee@jbnu.ac.kr

2014-05-12

We examined the electrooptical properties of a nematic liquid crystal (LC) sample whose substrates were coated with a mixture of carbon nanotube (CNT) and polyimide (PI). The relaxation time of the sample coated with 1.5 wt. % CNT mixture was about 35% reduced compared to the pure polyimide sample. The elastic constant and the order parameter of the CNT-mixture sample were increased and the fast relaxation of LC could be approximated to the mean-field theory. We found the CNT-mixed polyimide formed more smooth surface than the pure PI from atomic force microscopy images, indicating the increased order parameter is related to themore » smooth surface topology of the CNT-polyimide mixture.« less

Performance of Partially Fluorinated Polyimide Insulation for Aerospace Applications

NASA Technical Reports Server (NTRS)

Hammoud, Ahmad N.; Stavnes, Mark W.; Ide, James R.; Muegge, ED

1995-01-01

Polyimide has been used extensively as the primary wiring insulation in commercial planes, military aircraft, and space vehicles due to its low weight, high service temperature, and good dielectric strength. New failure modes, however, have been associated with the use of polyimide because of the susceptibility of the insulation to pyrolization and arc tracking. A new wiring construction utilizing partially fluorinated polyimide insulation has been tested and compared with the standard military polyimide wire. Electrical properties which were investigated include AC corona inception and extinction voltages (sea level and 60,000 feet), time/current to smoke, and wire fusing time. The two constructions were also characterized in terms of their mechanical properties including abrasion resistance, dynamic cut through, and notch propagation. These test efforts and the results obtained are presented and discussed.

Performance of partially fluorinated polyimide insulation for aerospace applications

NASA Astrophysics Data System (ADS)

Hammoud, Ahmad N.; Stavnes, Mark W.; Ide, James R.; Muegge, Ed

1995-08-01

Polyimide has been used extensively as the primary wiring insulation in commercial planes, military aircraft, and space vehicles due to its low weight, high service temperature, and good dielectric strength. New failure modes, however, have been associated with the use of polyimide because of the susceptibility of the insulation to pyrolization and arc tracking. A new wiring construction utilizing partially fluorinated polyimide insulation has been tested and compared with the standard military polyimide wire. Electrical properties which were investigated include AC corona inception and extinction voltages (sea level and 60,000 feet), time/current to smoke, and wire fusing time. The two constructions were also characterized in terms of their mechanical properties including abrasion resistance, dynamic cut through, and notch propagation. These test efforts and the results obtained are presented and discussed.

Evaluation of colorless polyimide film for thermal control coating applications

NASA Technical Reports Server (NTRS)

St.clair, A. K.; Slemp, W. S.

1985-01-01

A series of essentially colorless aromatic polyimide films was synthesized and characterized with the objective of obtaining maximum optical transparency for applications in space. Optical transparency is a requirement for high performance polymeric films used in second surface mirror coatings on thermal control systems. The intensity in color of aromatic polyimide films was lowered by reducing the electronic interaction between chromophoric centers in the polymer molecular structure and by using highly purified monomers. The resulting lightly colored to colorless polyimide films were characterized by UV-visible and infrared spectroscopy before and after exposure to 300 equivalent solar hours UV irradiation and varying doses of 1 MeV electron irradiation. After irradiation, the films were found to be 2 to 2.5 times more transparent than commercial polyimide film of the same thickness.

Surface characterization of LDEF materials

NASA Astrophysics Data System (ADS)

Wightman, J. P.; Grammer, Holly Little

1993-10-01

The NASA Long Duration Exposure Facility (LDEF), a passive experimental satellite, was placed into low-Earth orbit by the Shuttle Challenger in Apr. 1984. The LDEF spent an unprecedented 69 months in space. The flight and recovery of the LDEF provided a wealth of information on the longterm space environmental effects of a variety of materials exposed to the low-Earth orbit environment. Surface characterization of LDEF materials included polymers, composites, thermal control paints, and aluminum. X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), scanning electron microscopy (SEM), and contact angle analysis were used to document changes in both the surface composition and surface chemistry of these materials. Detailed XPS analysis of the polymer systems, such as Kapton, polyimide polysiloxane copolymers, and fluorinated ethylene propylene thermal blankets on the backside of the LDEF revealed significant changes in both the surface composition and surface chemistry as a result of exposure to the low-Earth orbit environment. Polymer systems such as Kapton, polyimide polysiloxane copolymers, and polysulfone showed a common trend of decreasing carbon content and increasing oxygen content with respect to the control sample. Carbon 1s curve fit XPS analysis of the composite samples, in conjunction with SEM photomicrographs, revealed significant ablation of the polymer matrix resin to expose the carbon fibers of the composite during exposure to the space environment. Surface characterization of anodized aluminum tray clamps, which were located at regular intervals over the entire LDEF frame, provided the first results to evaluate the extent of contamination with respect to position on the LDEF. The XPS results clearly showed that the amount and state of both silicon and fluorine contamination were directly dependent upon the position of the tray clamp on the LDEF.

High-Temperature Adhesive Strain Gage Developed

NASA Technical Reports Server (NTRS)

Pereira, J. Michael; Roberts, Gary D.

1997-01-01

Researchers at the NASA Lewis Research Center have developed a unique strain gage and adhesive system for measuring the mechanical properties of polymers and polymer composites at elevated temperatures. This system overcomes some of the problems encountered in using commercial strain gages and adhesives. For example, typical commercial strain gage adhesives require a postcure at temperatures substantially higher than the maximum test temperature. The exposure of the specimen to this temperature may affect subsequent results, and in some cases may be higher than the glass-transition temperature of the polymer. In addition, although typical commercial strain gages can be used for short times at temperatures up to 370 C, their long-term use is limited to 230 C. This precludes their use for testing some high-temperature polyimides near their maximum temperature capability. Lewis' strain gage and adhesive system consists of a nonencapsulated, unbacked gage grid that is bonded directly to the polymer after the specimen has been cured but prior to the normal postcure cycle. The gage is applied with an adhesive specially formulated to cure under the specimen postcure conditions. Special handling, mounting, and electrical connection procedures were developed, and a fixture was designed to calibrate each strain gage after it was applied to a specimen. A variety of tests was conducted to determine the performance characteristics of the gages at elevated temperatures on PMR-15 neat resin and titanium specimens. For these tests, which included static tension, thermal exposure, and creep tests, the gage and adhesive system performed within normal strain gage specifications at 315 C. An example of the performance characteristics of the gage can be seen in the figure, which compares the strain gage measurement on a polyimide specimen at 315 C with an extensometer measurement.

Surface characterization of LDEF materials

NASA Technical Reports Server (NTRS)

Wightman, J. P.; Grammer, Holly Little

1993-01-01

The NASA Long Duration Exposure Facility (LDEF), a passive experimental satellite, was placed into low-Earth orbit by the Shuttle Challenger in Apr. 1984. The LDEF spent an unprecedented 69 months in space. The flight and recovery of the LDEF provided a wealth of information on the longterm space environmental effects of a variety of materials exposed to the low-Earth orbit environment. Surface characterization of LDEF materials included polymers, composites, thermal control paints, and aluminum. X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), scanning electron microscopy (SEM), and contact angle analysis were used to document changes in both the surface composition and surface chemistry of these materials. Detailed XPS analysis of the polymer systems, such as Kapton, polyimide polysiloxane copolymers, and fluorinated ethylene propylene thermal blankets on the backside of the LDEF revealed significant changes in both the surface composition and surface chemistry as a result of exposure to the low-Earth orbit environment. Polymer systems such as Kapton, polyimide polysiloxane copolymers, and polysulfone showed a common trend of decreasing carbon content and increasing oxygen content with respect to the control sample. Carbon 1s curve fit XPS analysis of the composite samples, in conjunction with SEM photomicrographs, revealed significant ablation of the polymer matrix resin to expose the carbon fibers of the composite during exposure to the space environment. Surface characterization of anodized aluminum tray clamps, which were located at regular intervals over the entire LDEF frame, provided the first results to evaluate the extent of contamination with respect to position on the LDEF. The XPS results clearly showed that the amount and state of both silicon and fluorine contamination were directly dependent upon the position of the tray clamp on the LDEF.

Manufacturing of REBCO coils strongly bonded to cooling members with epoxy resin aimed at its application to Maglev

NASA Astrophysics Data System (ADS)

Mizuno, Katsutoshi; Ogata, Masafumi; Hasegawa, Hitoshi

2014-11-01

The REBCO coated conductor has been attracted attention because of its high current density in the presence of high magnetic field. If the coated conductor is applied to Maglev, the operational temperature of the on-board magnets will be over 40 K and energy consumption of cryocoolers will be reduced. That high operational temperature also means the absence of liquid helium. Therefore, reliable thermal coupling is desirable for cooling the coils. We propose an epoxy impregnated REBCO coil co-wound with PTFE tape. While the PTFE tape prevents the performance degradation of the coil, the epoxy resin bonds the coil to cooling members. We carried out three experiments to confirm that the coil structure which we propose has robust thermal coupling without the degradation. First, thermal resistances of paraffin and epoxy were measured varying the temperature from room temperature to 10 K. The measurement result indicates that paraffin has a risk of losing thermal coupling during cooling down. In another experiment, PTFE (polytetrafluoroethylene) tape insulator prevented performance degradation of a small epoxy impregnated REBCO coil, while another REBCO coil with polyimide tape showed clear performance degradation. Finally, we produced a racetrack REBCO coil with the same outer dimension as a Maglev on-board magnet coil. Although the racetrack coil was installed in a GFRP coil case and tightly bonded to the case by epoxy impregnation, any performance degradation was not observed.

Design, fabrication and test of graphite/polymide composite joints and attachments: Summary

NASA Technical Reports Server (NTRS)

Cushman, J. B.; Mccleskey, S. F.; Ward, S. H.

1983-01-01

The design, analysis and testing performed to develop four types of graphite/polyimide (Gr/PI) bonded and bolted composite joints for lightly loaded control surfaces on advanced space transportation systems that operate at temperatures up to 561K (550 F) are summarized. Material properties and 'small specimen' tests were conducted to establish design data and to evaluate specific design details. 'Static discriminator' tests were conducted on preliminary designs to verify structural adequacy. Scaled up specimens of the final joint designs, representative of production size requirements, were subjected to a series of static and fatigue tests to evaluate joint strength. Effects of environmental conditioning were determined by testing aged (125 hours 589K (600 F)) and thermal cycled (116K to 589K (-250 F to 600 F), 125 times) specimens. It is concluded Gr/PI joints can be designed and fabricated to carry the specified loads. Test results also indicate a possible resin loss or degradation of laminates after exposure to 589K (600 F) for 125 hours.

The development of an alternative thermoplastic powder prepregging technique

NASA Technical Reports Server (NTRS)

Ogden, A. L.; Hyer, M. W.; Wilkes, G. L.; Loos, A. C.

1992-01-01

An alternative powder prepregging technique is discussed that is based on the deposition of powder onto carbon fibers that have been moistened using an ultrasonic humidifier. The dry fiber tow is initially spread to allow a greater amount of the fiber surface to be exposed to the powder, thus ensuring a significant amount of intimate contact between the fiber and the matrix. Moisture in the form of ultrafine water droplets is then deposited onto the spread fiber tow. The moisture promotes adhesion to the fiber until the powder can be tacked to the fibers by melting. Powdered resin is then sieved onto the fibers and then tacked onto the fibers by quick heating in a convective oven. This study focuses on the production of prepregs and laminates made with LaRC-TPI (thermoplastic polyimide) using this process. Although the process appears to be successful, early evaluation was hampered by poor interfacial adhesion. The adhesion problem, however, seems to be the result of a material system incompatibility, rather than being influenced by the process.

Effect of protective coating on microhardness of a new glass ionomer cement: Nanofilled coating versus unfilled resin

PubMed Central

Faraji, Foad; Heshmat, Haleh; Banava, Sepideh

2017-01-01

Background and Objectives: EQUIATM is a new gastrointestinal (GI) system with high compressive strength, surface microhardness (MH), and fluoride release potential. This in vitro study aimed to assess the effect of aging and type of protective coating on the MH of EQUIATM GI cement. Materials and Methods: A total of 30 disc-shaped specimens measuring 9 mm in diameter and 2 mm in thickness were fabricated of EQUIATM GI and divided into three groups of G-Coat nanofilled coating (a), no coating (b) and margin bond (c). The Vickers MH value of specimens was measured before (baseline) and at 3 and 6 months after water storage. Data were analyzed using repeated measures ANOVA. Results: Group B had significantly higher MH than the other two groups at baseline. Both G-Coat and margin bond increased the surface MH of GI at 3 and 6 months. The MH values of G-Coat and margin bond groups did not significantly increase or decrease between 3 and 6 months. Conclusion: The increase in MH was greater in the G-Coat compared to the margin bond group in the long-term. Clinically, margin bond may be a suitable alternative when G-Coat is not available. PMID:29259364

Silicone Coating on Polyimide Sheet

NASA Technical Reports Server (NTRS)

Park, J. J.

1985-01-01

Silicone coatings applied to polyimide sheeting for variety of space-related applications. Coatings intended to protect flexible substrates of solar-cell blankets from degradation by oxygen atoms, electrons, plasmas, and ultraviolet light in low Earth orbit and outer space. Since coatings are flexible, generally useful in forming flexible laminates or protective layers on polyimide-sheet products.

Dimensionally Stable Ether-Containing Polyimide Copolymers

NASA Technical Reports Server (NTRS)

Fay, Catharine C. (Inventor); St.Clair, Anne K. (Inventor)

1999-01-01

Novel polyimide copolymers containing ether linkages were prepared by the reaction of an equimolar amount of dianhydride and a combination of diamines. The polyimide copolymers described herein possess the unique features of low moisture uptake, dimensional stability, good mechanical properties, and moderate glass transition temperatures. These materials have potential application as encapsulants and interlayer dielectrics.

Polyimide Aerogels with Three-Dimensional Cross-Linked Structure

NASA Technical Reports Server (NTRS)

Meador, Mary Ann B. (Inventor)

2016-01-01

A method for creating a three dimensional cross-linked polyimide structure includes dissolving a diamine, a dianhydride, and a triamine in a solvent, imidizing a polyamic acid gel by heating the gel, extracting the gel in a second solvent, supercritically drying the gel, and removing the solvent to create a polyimide aerogel.

Reinforced Thermoplastic Polyimide with Dispersed Functionalized Single Wall Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Lebron-Colon, Marisabel; Meador, Michael A.; Gaier, James R.; Sola, Francisco; Scheiman, Daniel A.; McCorkle, Linda S.

2010-01-01

Molecular pi-complexes were formed from pristine HiPCO single-wall carbon nanotubes (SWCNTs) and 1-pyrene- N-(4- N'-(5-norbornene-2,3-dicarboxyimido)phenyl butanamide, 1. Polyimide films were prepared with these complexes as well as uncomplexed SWCNTs and the effects of nanoadditive addition on mechanical, thermal, and electrical properties of these films were evaluated. Although these properties were enhanced by both nanoadditives, larger increases in tensile strength and thermal and electrical conductivities were obtained when the SWCNT/1 complexes were used. At a loading level of 5.5 wt %, the Tg of the polyimide increased from 169 to 197 C and the storage modulus increased 20-fold (from 142 to 3045 MPa). The addition of 3.5 wt % SWCNT/1 complexes increased the tensile strength of the polyimide from 61.4 to 129 MPa; higher loading levels led to embrittlement and lower tensile strengths. The electrical conductivities (DC surface) of the polyimides increased to 1 x 10(exp -4) Scm(exp -1) (SWCNT/1 complexes loading level of 9 wt %). Details of the preparation of these complexes and their effects on polyimide film properties are discussed.

Fabrication and evaluation of dispersed-Ag nanoparticles-in-polyimide thin films

NASA Astrophysics Data System (ADS)

Sonehara, Makoto; Watanabe, Yuki; Yamaguchi, Sota; Kato, Takanori; Yoshisaku, Yasuaki; Sato, Toshiro; Itoh, Eiji

2017-10-01

A thin-film common-mode filter (TF-CMF) for cell phones in the UHF band was fabricated and evaluated. The TF-CMF consisted of multiple metal-insulator-metal (MIM) capacitors and inductors. The sizes of the 0.70-1.0 GHz band-type and 1.8-2.0 GHz band-type TF-CMFs are 1,140 × 1,260 × 10.5 µm3, and 1,060 × 1,060 × 10.5 µm3, respectively. The footprint in both types of TF-CMFs is over 1 mm2. In order to miniaturize the TF-CMF, we proposed to change a polyimide-only to a polyimide with dispersed Ag nanoparticles with high permittivity in the insulator layer for the MIM capacitor of the TF-CMF. A polyimide (\\text{polyimide precursor}:\\text{toluene with dispersed Ag nanoparticles} = 100:1) thin film with dispersed high-density Ag nanoparticles has a relative permittivity of about 8, which is twice as high as that of the polyimide-only thin film. If the capacitance and distance between electrodes are the same, then the capacitor footprint may be halved.

Analysis of the Effect of Surface Modification on Polyimide Composites Coated with Erosion Resistant Materials

NASA Technical Reports Server (NTRS)

Ndalama, Tchinga; Hirschfeld, Deidre; Sutter, James K. (Technical Monitor)

2003-01-01

The aim of this research is to enhance performance of composite coatings through modification of graphite-reinforced polyimide composite surfaces prior to metal bond coat/ hard topcoat application for use in the erosive and/or oxidative environments of advanced engines. Graphite reinforced polyimide composites, PMR-15 and PMR-II-50, formed by sheet molding and pre-pregging will be surface treated, overlaid with a bond coat and then coated with WC-Co. The surface treatment will include cleaning, RF plasma or ultraviolet light- ozone etching, and deposition of SiO(x) groups. These surface treatments will be studied in order to investigate and improve adhesion and oxidation resistance. The following panels were provided by NASA-Glenn Research Center(NASA-GRC): Eight compression molded PMR-II-50; 6 x 6 x 0.125 in. Two vacuum-bagged PMR-II-50; 12 x 12 x 0.125 in. Eight compression molded PMR-15; 6 x 6 x 0.125 in. One vacuum-bagged PMR-15; 12 x 12 x 0.125 in. All panels were made using a 12 x 12 in. T650-35 8HS (3K-tow) graphite fabric. A diamond-wafering blade, with deionized water as a cutting fluid, was used to cut PMR-II-50 and PMR-15 panels into 1 x 1 in. pieces for surface tests. The panel edges exhibiting delamination were used for the preliminary surface preparation tests as these would be unsuitable for strength and erosion testing. PMR-15 neat resin samples were also provided by NASA GRC. Surface profiles of the as-received samples were determined using a Dektak III Surface profile measuring system. Two samples of compression molded PMR-II-50 and PMR-15, vacuum-bagged PMR-II-50 and PMR-15 were randomly chosen for surface profile measurement according to ANSI/ASME B46.1. Prior to each measurement, the samples were blasted with compressed air to remove any artifacts. Five 10 mm-long scans were made on each sample. The short and long wavelength cutoff filter values were set at 100 and 1000 m, diamond stylus radius was 12.5 microns. Table 1 is a summary of the arithmetic average roughness (Ra) and waviness (Wa) for the composite surfaces.

Evaluation of colorless polyimide film for thermal control coating applications

NASA Technical Reports Server (NTRS)

St. Clair, A. K.; Slemp, W. S.

1985-01-01

A series of essentially colorless aromatic polyimide films has been synthesized and characterized with the objective of obtaining maximum optical transparency for applications in space. Optical transparency is a requirement for high performance polymeric films used in second surface mirror coatings on thermal control systems. The intensity in color of aromatic polyimide films was lowered by reducing the electronic interaction between chromophoric centers in the polymer molecular structure and by using highly purified monomers. The resulting lightly colored to colorless polyimide films have been characterized by UV-visible and infrared spectroscopy before and after exposure to 300 equivalent solar hours UV irradiation and varying doses of 1 MeV electron irradiation. After irradiation, the films were found to be 2 to 2.5 times more transparent than commercial polyimide film of the same thickness.

Polyimides and Process for Preparing Polyimides Having Thermal-Oxidative Stability

NASA Technical Reports Server (NTRS)

Meador, Mary Ann B. (Inventor)

2001-01-01

Polyimides and the process for preparing polyimides having improved thermal-oxidative stability derived from the polymerization of effective amounts of one or more of the polyamines such as the aromatic diamines, one or more of the tetracarboxylic dianhydrides and a novel dicarboxylic endcap having formula with an R1 group of either hydrogen or an alkyl radical of one to four carbons, an R2 group of either OH, NH2, F, or Cl radical, an R3 group of either H, OH, NH2, F, Cl or an alkylene radical, an R4 group of either an alkyl, aryl, aryloxy, nitro, F, or Cl radical, and/or an R5 group of either H, alkyl, aryl, alkoxy, aryloxy, nitro, F, or Cl radical. The polyimides are useful particularly in the preparation of prepegs and PMR composites.

Polyimide Aerogel Thin Films

NASA Technical Reports Server (NTRS)

Meador, Mary Ann; Guo, Haiquan

2012-01-01

Polyimide aerogels have been crosslinked through multifunctional amines. This invention builds on "Polyimide Aerogels With Three-Dimensional Cross-Linked Structure," and may be considered as a continuation of that invention, which results in a polyimide aerogel with a flexible, formable form. Gels formed from polyamic acid solutions, end-capped with anhydrides, and cross-linked with the multifunctional amines, are chemically imidized and dried using supercritical CO2 extraction to give aerogels having density around 0.1 to 0.3 g/cubic cm. The aerogels are 80 to 95% porous, and have high surface areas (200 to 600 sq m/g) and low thermal conductivity (as low as 14 mW/m-K at room temperature). Notably, the cross-linked polyimide aerogels have higher modulus than polymer-reinforced silica aerogels of similar density, and can be fabricated as both monoliths and thin films.

Advanced Polymers Containing the Phenyltrifluoroethylidene Connecting Group

NASA Technical Reports Server (NTRS)

Alstron, William B.; Sivko, Gloria S.

2006-01-01

A new, lower cost fluorinated dianhydride based on the phenyltrifluoroethylidene (3F) connecting linkage was invented by the principal author in the early 1980's. New 3F condensation and addition cured polyimides were synthesized with the newly discovered 3F dianhydride and the previously known 3F diamine. As controls, polyimides based on the somewhat analogous higher cost hexafluoroisopropylidene (6F) linkage were also prepared. The short term thermal oxidative stability (TOS), determined by thermal gravimetric analysis (TGA), and the glass transition temperatures (Tg) of 3F dianhydride polyimides were found to be similar to 6F dianhydride polyimides, but the Tg was slightly higher for 3F diamine polyimides than 6F diamine polyimides. Unfortunately, in real time testing, long term TOS of 3F polymers was clearly inferior to 6F polymers. This was due to a 3 to 5 fold greater rate of loss of trifluoromethyl group from 3F versus 6F linkages. However, at shorter times or lower temperatures, 3F TOS was almost comparable to 6F TOS. The wide scope of the 3F technology was also demonstrated to have distinct unique advantages over 6F technology through the use of the 3F pendant phenyl ring as a synthetic site to introduce other functional groups. These groups have been used for the control or modification of polymer properties; an advantage lacking within 6F technology. The synthetic ease by which 3F can be introduced into various types of monomers has lead to the explosion of advanced 3F polyimides and other high performance advanced 3F polymers in the prior decade of 3F polymer literature as cited herein; covering polyimides, substituted polyimides, at least ten types of nonpolyimide 3F polymer modifications, and also the government's nine 3F U.S. patents and corporations' nine 3F U.S. patents.

Low-Dielectric Polyimides

NASA Technical Reports Server (NTRS)

St. Clair, Anne K.; St. Clair, Terry L.; Winfree, William P.; Emerson, Bert R., Jr.

1989-01-01

New process developed to produce aromatic condensation polyimide films and coatings having dielectric constants in range of 2.4 to 3.2. Materials better electrical insulators than state-of-the-art commercial polyimides. Several low-dielectric-constant polyimides have excellent resistance to moisture. Useful as film and coating materials for both industrial and aerospace applications where high electrical insulation, resistance to moisture, mechanical strength, and thermal stability required. Applicable to production of high-temperature and moisture-resistance adhesives, films, photoresists, and coatings. Electronic applications include printed-circuit boards, both of composite and flexible-film types and potential use in automotive, aerospace, and electronic industries.

Fire-resistant phosphorus containing polyimides and copolyimides

NASA Technical Reports Server (NTRS)

Mikroyannidis, J. A. (Inventor)

1985-01-01

Phosphorus-containing polyimides and copolyimides are synthesized in a two-step polycondensation reaction from 1- (diorganooxyphosphonl)methly 2,4- and 2,6-diaminobenzenes and tetracarboxylic anhydride. The diorgano position of the diorganooxyphosphonyl group includes alkyl, such as ethyl, substituted alkyl, such as 2-chloroethyl, and aryl such as phenyl. The tetracarboxylic anhydries include compounds such as pyrometallitic dianhydride and benzophenone tetracarboxylic dianhydride. The glass transition temperature (Tg) of the polyimides is reduced by incorporation of the (dialkoxyphosphonyl)methyl groups. The phosphorus-containing copolyimides show a considerably higher degree of fire-resistance as compared to that of the corresponding common polyimides.

The hydrolysis of polyimides

NASA Technical Reports Server (NTRS)

Hoagland, P. D.; Fox, S. W.

1973-01-01

Thermal polymerization of aspartic acid produces a polysuccinimide (I), a chain of aspartoyl residues. An investigation was made of the alkaline hydrolysis of the imide rings of (I) which converts the polyimide to a polypeptide. The alkaline hydrolysis of polyimides can be expected to be kinetically complex due to increasing negative charge generated by carboxylate groups. For this reason, a diimide, phthaloyl-DL-aspartoyl-beta-alanine (IIA) was synthesized for a progressive study of the hydrolysis of polyimides. In addition, this diimide (IIA) can be related to thalidomide and might be expected to exhibit similar reactivity during hydrolysis of the phthalimide ring.

Polyimides containing pendent trifluoromethyl groups

NASA Technical Reports Server (NTRS)

Havens, S. J.; Hergenrother, P. M.

1993-01-01

Several new polyimides containing trifluoromethyl groups were prepared from the reaction of various aromatic dianhydrides and two new diamines containing trifluoromethyl groups, 4,4'-bis(3-amino-5-trifluoromethylphenoxy)biphenyl and l,4-bis(3-amino-5-trifluoromethylphenoxy)benzene. The diamines were prepared from the aromatic nucleophilic displacement of the disodium salts of 4,4'-biphenol or hydroquinone with 3,5-dinitrobenzotrifluoride followed by hydrogenation of the resultant dinitro compounds. The thermally cured polyimides exhibited glass transition temperatures between 186 and 262 C. By thermogravimetric analysis, the polyimides exhibited 5 percent weight losses at 484-527 C in nitrogen and 452-506 C in air.

Polyimides: Tribological properties and their use as lubricants

NASA Technical Reports Server (NTRS)

Fusaro, R. L.

1982-01-01

Friction, wear, and wear mechanisms of several different polyimide films, solid bodies, composites, and bonded solid lubricant films are compared and discussed. In addition, the effect of such parameters as temperatures, type of atmosphere, contact stress, and specimen configuration are investigated. A friction and wear transition occurs in some polyimides at elevated temperatures and this transition is related to molecular relaxations that occur in polyimides. Friction and wear data from an accelerated test (pin-on-disk) are compared to similar data from an end use test device (plain spherical bearing), and to other polymers investigated in a similar geometry.

Structural Health Monitoring of Composite Wound Pressure Vessels

NASA Technical Reports Server (NTRS)

Grant, Joseph; Kaul, Raj; Taylor, Scott; Jackson, Kurt; Myers, George; Sharma, A.

2002-01-01

The increasing use of advanced composite materials in the wide range of applications including Space Structures is a great impetus to the development of smart materials. Incorporating these FBG sensors for monitoring the integrity of structures during their life cycle will provide valuable information about viability of the usage of such material. The use of these sensors by surface bonding or embedding in this composite will measure internal strain and temperature, and hence the integrity of the assembled engineering structures. This paper focuses on such a structure, called a composite wound pressure vessel. This vessel was fabricated from the composite material: TRH50 (a Mitsubishi carbon fiber with a 710-ksi tensile strength and a 37 Msi modulus) impregnated with an epoxy resin from NEWPORT composites (WDE-3D-1). This epoxy resin in water dispersed system without any solvents and it cures in the 240-310 degrees F range. This is a toughened resin system specifically designed for pressure applications. These materials are a natural fit for fiber sensors since the polyimide outer buffer coating of fiber can be integrated into the polymer matrix of the composite material with negligible residual stress. The tank was wound with two helical patterns and 4 hoop wraps. The order of winding is: two hoops, two helical and two hoops. The wall thickness of the composite should be about 80 mil or less. The tank should burst near 3,000 psi or less. We can measure the actual wall thickness by ultrasonic or we can burst the tank and measure the pieces. Figure 1 shows a cylinder fabricated out of carbon-epoxy composite material. The strain in different directions is measured with a surface bonded fiber Bragg gratings and with embedded fiber Bragg gratings as the cylinder is pressurized to burst pressures. Figure 2 shows the strain as a function of pressure of carbon-epoxy cylinder as it is pressurized with water. Strain is measured in different directions by multiple gratings oriented in both axial and hoops directions.

Functionalized Silk Materials

DTIC Science & Technology

2010-06-10

properties, such as toughness, biocompatibility and biodegrability. Trends in spider silk-like block copolymer secondary structure and assembly behavior...to construct transistors on ultrathin sheets of polyimide . Briefly, the doped silicon nanomembranes were transfer printed onto a film of polyimide ...layer of polyimide was used to encapsulate the active devices. Dry etching the polymer layers completed the fabrication of an array of isolated

Composition and Process for Retarding the Premature Aging of PMR Monomer Solutions and PMR Prepegs

NASA Technical Reports Server (NTRS)

Alston, William B. (Inventor); Gahn, Gloria S. (Inventor)

2000-01-01

Polyimides are derived from solutions of at least one low-boiling organic solvent, e.g. isopropanol containing a mixture of polyimide-forming monomers. The monomeric solutions have an extended shelf life at ambient (room) temperatures as high as 80 C, and consist essentially of a mixture of monoalkyl ester-acids, alkyl diester-diacids and aromatic polyamines wherein the alkyl radicals of the esteracids are derived from lower molecular weight aliphatic secondary alcohols having 3 to 5 carbon atoms per molecule such as isopropanol, secondary butanol, 2-methyl-3-butanol, 2 pentanol or 3-pentanol. The solutions of the polyimide-forming monomers have a substantially improved shelf-life and are particularly useful in the aerospace and aeronautical industry for the preparation of polyimide reinforced fiber composites such as the polyimide cured carbon composites used in jet engines, missiles, and for other high temperature applications.

Tribological properties and thermal stability of various types of polyimide films

NASA Technical Reports Server (NTRS)

Fusaro, R. L.

1981-01-01

Thermal exposure experiments at 315 and 350 C were conducted on seven different types of polyimide films to determine which was the most thermally stable and adherent. The polyimides were ranked according to the rate at which they lost weight and how well they adhere to the metallic substrate. Friction and wear experiments were conducted at 25 C (room temperature) on films bonded to 440C HT stainless steel. Friction, film wear rates, wear mechanisms, and transfer films of the seven films were investigated and compared. The polyimides were found to fall into two groups as far as friction and wear properties were concerned. Group one had lower friction but an order of magnitude higher film wear rate than did group two. The wear mechanism was predominately adhesive, but the size of the wear particles were larger for group one polyimides.

Tribological properties and thermal stability of various types of polyimide films

NASA Technical Reports Server (NTRS)

Fusaro, R. L.

1981-01-01

Thermal exposure experiments at 315 and 350 C were conducted on seven different types of polyimide films to determine which was the most thermally stable and adherent. The polyimides were ranked according to the rate of which they lost weight and how well they adhered to the metallic substrate. Friction and wear experiments were conducted at 25 C (room temperature) on films bonded to 440C HT stainless steel. Friction, film wear rates, wear mechanisms, and transfer films of the seven films were investigated and compared. The polyimides were found to fall into two groups as far as friction and wear properties were concerned. Group I had lower friction but an order of magnitude higher film wear rate than did group II. The wear mechanism was predominately adhesive, but the size of the wear particles was larger for group I polyimides.

Surface Modification of Polyimide for Improving Adhesion Strength by Inductively Coupled Plasma

NASA Astrophysics Data System (ADS)

Byun, Tae Joon; Kim, Sung Il; Kim, Youn Joon; Choi, Yoon Suk; Choi, In Sik; Setsuhara, Yuichi; Geon Han, Jeon

2009-08-01

This study examined the effect of an inductively coupled plasma (ICP) treatment using an argon and helium gas mixture on the adhesion between polyimide and a copper film. Optical emission spectroscopy (OES) of the ICP revealed the emission intensity of helium and argon at various intensities with the helium mixing ratio. The treated polyimide surface was analyzed using a contact angle analyzer, Atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The contact angle and RMS roughness ranged from 66 to 31° and 2.3 to 4.1 nm, respectively. XPS showed an increase in C-O bonding. The highest peel strength was 0.43 kgf/cm at a 40% of helium mixing ratio, which contained the highest level of activate species. Overall, an ICP treatment of a polyimide surface with a 40% helium gas mixture improves the adhesion strength between copper and polyimide significantly.

Study of the technics of coating stripping and FBG writing on polyimide fiber

NASA Astrophysics Data System (ADS)

Song, ZhiQiang; Qi, HaiFeng; Ni, JiaSheng; Wang, Chang

2017-10-01

Compared with ordinary optical fiber, polyimide fiber has the characteristics of high temperature resistance and high strength, which has important application in the field of optical fiber sensing. The common methods of polyimide coating stripping were introduced in this paper, including high temperature stripping, chemical stripping and arc ablation. In order to meet the requirements of FBG writing technology, a method using argon ion laser ablation coating was proposed. The method can precisely control the stripping length of the coating and completely does not affect the tensile strength of the optical fiber. According to the experiment, the fabrication process of polyimide FBG is stripping-hydrogen loadingwriting. Under the same conditions, 10 FBG samples were fabricated with good uniformity of wavelength bandwidth and reflectivity. UV laser ablation of polyimide coating has been proved to be a safe, reliable and efficient method.

High-Performance Polyimide Powder Coatings

NASA Technical Reports Server (NTRS)

2008-01-01

Much of the infrastructure at Kennedy Space Center and other NASA sites has been subjected to outside weathering effects for more than 40 years. Because much of this infrastructure has metallic surfaces, considerable effort is continually devoted to developing methods to minimize the effects of corrosion on these surfaces. These efforts are especially intense at KSC, where offshore salt spray and exhaust from Solid Rocket Boosters accelerate corrosion. Coatings of various types have traditionally been the choice for minimizing corrosion, and improved corrosion control methods are constantly being researched. Recent work at KSC on developing an improved method for repairing Kapton (polyimide)-based electrical wire insulation has identified polyimides with much lower melting points than traditional polyimides used for insulation. These lower melting points and the many other outstanding physical properties of polyimides (thermal stability, chemical resistance, and electrical properties) led us to investigate whether they could be used in powder coatings.

Non-flammable polyimide materials for aircraft and spacecraft applications

NASA Technical Reports Server (NTRS)

Gagliani, J.; Supkis, D. E.

1979-01-01

Recent developments in polyimide chemistry show promise for producing materials with very low flammability and a wide range of mechanical properties. Polyimide foams can be synthesized to provide fire safety without detectable formation of smoke or toxic byproducts below 204 C (400 F), thus avoiding an environment which is lethal to human habitation. This work has been and is currently being performed under development programs, the objective of which is to provide cost effective processes for producing thermally stable, polyimide flexible resilient foams, thermal-acoustical insulating materials, rigid low density foam panels, and high strength foam structures. The chemical and physical properties demonstrated by these materials represent a technological advancement in the art of thermally stable polyimide polymers which are expected to insure fire protection of structures and components used in air transportation and space exploration. Data compiled to date on thermal, physical and functional properties of these materials are presented.

Investigation of Aromatic/Aliphatic Polyimides as Dispersants for Single Wall Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Delozier, Donavon M.; Watson, Kent A.; Smith, Joseph G., Jr.; Clancy, Thomas C.; Connell, John W.

2006-01-01

Novel aromatic/aliphatic polyimides were prepared from 2,7-diamino-9,9'- dioctylfluorene (AFDA) and aromatic dianhydrides. Upon investigating the effectiveness of these polyimides for dispersing single wall carbon nanotubes (SWNTs) in solution, three were discovered to disperse SWNTs in N,N-dimethylacetamide (DMAc). Two of these polyimides, one from 3,3',4,4'-oxydiphthalic anhydride (ODPA) and one from symmetric 3,3',4,4'-biphenyltetracarboxylic dianhydride (s-BPDA), were used to prepare nanocomposites. Homogeneous polyimide/SWNT suspensions from both polymers were used in the preparation of films and fibers containing up to 1 wt% SWNTs. The samples were thermally treated to remove residual solvent and the films were characterized for SWNT dispersion by optical and high resolution scanning electron microscopy (HRSEM). Electrical and mechanical properties of the films were also determined. Electrospun fibers were examined by HRSEM to characterize SWNT alignment and orientation.

Microelectrodes with Three-Dimensional Structures for Improved Neural Interfacing

DTIC Science & Technology

2001-10-25

highly xible bio-interfaces [2]. Polyimides combine excellent ectrical and mechanical characteristics with biocompatibility ], and are well known in...excellent biocompatibility , polyimide -based electrodes promise for fabrication of long-term implants for the use in prostheses. The flexible structures...R. R. Richardson, J. A. Miller, and W. M. Reichert, " Polyimides as Biomaterials - Preliminary Biocompatibility Testing," Biomaterials, vol. 14, pp

Processable Aromatic Polyimide Thermoplastic Blends

NASA Technical Reports Server (NTRS)

Baucom, Robert M; Johnston, Norman J.; St. Clair, Terry L.; Nelson, James B.; Gleason, John R.; Proctor, K. Mason

1988-01-01

Method developed for preparing readily-processable thermoplastic polyimides by blending linear, high-molecular-weight, polyimic acid solutions in ether solvents with ultrafine, semicrystalline, thermoplastic polyimide powders. Slurries formed used to make prepregs. Consolidation of prepregs into finsihed composites characterized by excellent melt flow during processing. Applied to film, fiber, fabric, metal, polymer, or composite surfaces. Used to make various stable slurries from which prepregs prepared.

LARC-TPI and new thermoplastic polyimides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yamaguchi, A.; Ohta, M.

1987-02-01

The LARC-TPI linear thermoplastic polyimide has been developed by NASA for high temperature adhesive applications in aerospace structures in the forms of varnish, films, powders, and prepregs. LARC-TPI improves adhesive processability and lowers glass transition temperature, while retaining mechanical, thermal and electrical properties inherent in the polyimides. It may be used as a structural adhesive for metals, composites, ceramics, and films. 8 references.

Characterization of a thermally imidized soluble polyimide film

NASA Technical Reports Server (NTRS)

Young, Philip R.; Davis, Judith R. J.; Chang, A. C.; Richardson, John N.

1989-01-01

A soluble aromatic poly(amic acid) film was converted to a soluble polyimide by staging at 25 deg intervals to 325 C and characterized at each interval by several analytical methods. The behavior observed was consistent with an interpretation that a reduction occurred in molecular weight of the poly(amic acid) during the initial stages of cure before the ultimate molecular weight was achieved as a polyimide. This interpretation was supported by the results of solution viscosity, gel permeation chromatography, low angle laser light scattering photometry and infrared spectroscopy analysis. The results serve to increase the fundamental understanding of how polyimides are thermally formed from poly(amic acids).

The mechanical properties of polyimide films after exposure to high pH

NASA Technical Reports Server (NTRS)

Croall, Catharine I.; St.clair, Terry L.

1992-01-01

Wiring failures linked to insulation damage have drawn much attention in the aerospace industry and concerns have developed regarding the stability and safety of polyimide insulated electrical wire. Several polyimides were selected for evaluation for resistance to degradation by various aqueous alkaline solutions. The polyimides under evaluation include commercially available films such as Kapton (tk), Apical (tk), LaRC(tk)-TPI, and Upilex(tk)R and S, as well as a number of experimental films prepared by NASA Langley. Thermally imidized films were studied for their retention of mechanical properties after exposure to high pH solutions under stressed conditions.

Effect of using polyimide capillaries during thermal experiments on the particle size distribution of supported Pt nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gámez-Mendoza, Liliana; Resto, Oscar; Martínez-Iñesta, María

2015-09-20

Kapton HN-type polyimide capillaries are commonly used as sample holders for transmission X-ray experiments at temperatures below 673 K because of their thermal stability, high X-ray transmittance and low cost. Using high-angle annular dark field scanning high-resolution transmission electron microscopy and thermogravimetric analysis, this work shows that using polyimide capillaries leads to the overgrowth of supported Pt nanoparticles during reduction at temperatures below the glass transition temperature (T g= 658 K) owing to an outgassing of water from the polyimide. Quartz capillaries were also studied and this overgrowth was not observed.

Propagation Characteristics of Finite Ground Coplanar Waveguide on Si Substrates With Porous Si and Polyimide Interface Layers

NASA Technical Reports Server (NTRS)

Ponchak, George E.; Itotia, Isaac K.; Drayton, Rhonda Franklin

2003-01-01

Measured and modeled propagation characteristics of Finite Ground Coplanar (FGC) waveguide fabricated on a 15 ohm-cm Si substrate with a 23 micron thick, 68% porous Si layer and a 20 micron thick polyimide interface layer are presented for the first time. Attenuation and effective permittivity as function of the FGC geometry and the bias between the center conductor and the ground planes are presented. It is shown that the porous Si reduces the attenuation by 1 dB/cm compared to FGC lines with only polyimide interface layers, and the polyimide on porous silicon demonstrates negligible bias dependence.

Highly optical transparency and thermally stable polyimides containing pyridine and phenyl pendant.

PubMed

Yao, Jianan; Wang, Chunbo; Tian, Chengshuo; Zhao, Xiaogang; Zhou, Hongwei; Wang, Daming; Chen, Chunhai

2017-01-01

In order to obtain highly optical transparency polyimides, two novel aromatic diamine monomers containing pyridine and kinky structures, 1,1-bis[4-(5-amino-2-pyridinoxy)phenyl]diphenylmethane (BAPDBP) and 1,1-bis[4-(5-amino-2-pyridinoxy)phenyl]-1-phenylethane (BAPDAP), were designed and synthesized. Polyimides based on BAPDBP, BAPDAP, 2,2-bis[4-(5-amino-2-pyridinoxy)phenyl]propane (BAPDP) with various commercial dianhydrides were prepared for comparison and structure-property relationships study. The structures of the polyimides were characterized by Fourier transform infrared (FT-IR) spectrometer, wide-angle X-ray diffractograms (XRD) and elemental analysis. Film properties including solubility, optical transparency, water uptake, thermal and mechanical properties were also evaluated. The introduction of pyridine and kinky structure into the backbones that polyimides presented good optical properties with 91-97% transparent at 500 nm and a low cut-off wavelength at 353-398 nm. Moreover, phenyl pendant groups of the polyimides showed high glass transition temperatures ( T g ) in the range of 257-281 °C. These results suggest that the incorporating pyridine, kinky and bulky substituents to polymer backbone can improve the optical transparency effectively without sacrificing the thermal properties.