Phenylethynyl terminated imide oligomers

NASA Technical Reports Server (NTRS)

Hergenrother, Paul M. (Inventor); Bryant, Robert G. (Inventor); Jensen, Brian J. (Inventor); Havens, Stephen J. (Inventor)

1995-01-01

Four phenylethynyl amine compounds - 3 and 4-aminophenoxy-4'-phenylethynylbenzophenone, and 3 and 4-amino-4'-phenylethynylbenzophenone - were readily prepared and were used to endcap imide oligomers. Phenylethynyl-terminated amide acid oligomers and phenylethynyl-terminated imide oligomers with various molecular weights and compositions were prepared and characterized. These oligomers were cured at 300 to 400 C to provide crosslinked polyimides with excellent solvent resistance, high strength and modulus, and good high temperature properties. Adhesive panels, composites, films, and moldings from these phenylethynyl terminated imide oligomers gave excellent mechanical performance.

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.

High T(g) Polyimides

NASA Technical Reports Server (NTRS)

Chuang, Kathy

2001-01-01

The use of high temperature polymer matrix composites in aerospace applications has expanded steadily over the past 30 years, due to the increasing demand of replacing metal parts with light weight composite materials for fuel efficiency and bigger payloads in the aircraft and the space transportation vehicles. Polyimide/carbon fiber composites, especially, have been regarded as major high temperature matrix materials, based on their outstanding performance in terms of heat resistance, high strength-to-weight ratio and property retention compared with epoxies (177 C/350 F) and bismaleimides (232 C/450 F). Traditional, then-neoplastic polyimides were prepared from dianhydrides and diamines in N-methyl-2-pyrrolidinone (NMP) at room temperature to form the polyamic acids, which were then imidized at 150 C to yield polyimides. However, the high-boiling solvent (NMP, BP= 202 C) is very difficult to remove, leading to the formation of voids during composite fabrication. In the early 1970's, PMR addition curing polyimides with reactive endcaps were developed at the Lewis Research Center (renamed NASA Glenn) to ensure the easy processing of imide oligomers in methanol during composite fabrication.

Novel poly(imide dioxime) sorbents: Development and testing for enhanced extraction of uranium from natural seawater

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

Das, Sadananda; Brown, Suree; Mayes, Richard T.

2016-04-09

We synthesized a new series of amidoxime-based polymer adsorbents at the Oak Ridge National Laboratory (ORNL) by electron beam induced grafting of acrylonitrile and itaconic acid onto polyethylene fiber. We also demonstrate hydroxylamine derivatives of poly(acrylonitrile) (PAN) moiety to possess two kinds of functional groups: open-chain amidoxime and cyclic imide dioxime. The open-chain amidoxime is shown to convert to imide dioxime on heat treatment in the presence of an aprotic solvent, like dimethylsulfoxide (DMSO). Furthermore, the formation of amidoxime and imide dioxime was confirmed by 13C CP-MAS spectra. The adsorbents were evaluated for uranium adsorption efficiency at ORNL with simulatedmore » seawater spiked with 8 ppm uranium and 5 gallon seawater in a batch reactor, and in flow-through columns with natural seawater at the Marine Science Laboratory (MSL) of Pacific Northwest National Laboratory (PNNL) at Sequim Bay, WA. The DMSO-heat-treated sorbents adsorbed uranium as high as 4.48 g-U/kg-ads. from seawater. Experimental evidence is presented that the poly(imide dioxime) is primarily responsible for enhanced uranium adsorption capacity from natural seawater. The conjugated system in the imide dioxime ligand possesses increased electron donation ability, which is believed to significantly enhance the uranyl coordination in seawater.« less

Characterization, liquid crystalline behavior, electrochemical and optoelectrical properties of new poly(azomethine)s and a poly(imide) with siloxane linkages

NASA Astrophysics Data System (ADS)

Iwan, Agnieszka; Schab-Balcerzak, Ewa; Pociecha, Damian; Krompiec, Michal; Grucela, Marzena; Bilski, Pawel; Kłosowski, Mariusz; Janeczek, Henryk

2011-11-01

New siloxane-containing poly(azomethine)s and a six-membered poly(imide) have been developed from siloxane-containing diamine with four different dialdehydes and 3,4,9,10-perylenetetracarboxylic dianhydride, and their thermotropic behavior, optoelectrical and electrochemical properties were examined. Mesomorphic behavior of the polymers was investigated via differential scanning calorimetry (DSC), polarizing optical microscopy (POM) and X-ray diffraction (WAXRD, SAXRD) studies. The electrochemical behavior of poly(azomethine)s and poly(imide) was studied by differential pulse voltammetry (DPV). The HOMO levels of these polymers were in the range of -5.13 to -5.90 eV. UV-vis properties of the polymers were investigated in solid state as thin films and in chloroform solution. Optical energy band gap ( Egopt.) was calculated from absorption spectra and absorption coefficients α. The photoluminescence properties (PL) of obtained polymers were studied in chloroform solution. The investigated poly(azomethine)s emitted blue light, while the poly(imide) emitted green light. The polymers were irradiated with a test dose of 1 Gy Co-60 gamma-rays to detect their thermoluminescence properties in the temperature range of 50-200 °C. Polymer monolayer (ITO/polymer/Al) and bulk heterojunction (BHJ) (ITO/polymer:PCBM/Al and ITO/PEDOT:PSS/polymer:PCBM/Al) devices were prepared with PAZ and PI used as active layers and I- U curves were measured in the dark and during irradiation with light (under illumination of 1000 W/m 2). Poly(azomethine)s were blended with [6,6]-phenyl C 61 butyric acid methyl ester (PCBM). Selected properties of the investigated polymers with siloxane linkages were compared with the polymers ( PAZ1a- PAZ3a, PIa) prepared from the same dialdehydes or dianhydride and poly(1,4-butanediol)bis(4-aminobenzoate).

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.

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.

Commercialization of LARC (TradeMark) -SI Polyimide Technology

NASA Technical Reports Server (NTRS)

Bryant, Robert G.

2011-01-01

LARC(TradeMark)-SI, Langley Research Center- Soluble Imide, was developed in 1992, with the first patent issuing in 1997, and then subsequent patents issued in 1998 and 2000. Currently, this polymer has been successfully licensed by NASA, and has generated revenues, at the time of this reporting, in excess of $1.4 million. The success of this particular polymer has been due to many factors and many lessons learned to the point that the invention, while important, is the least significant part in the commercialization of this material. Commercial LARC(TradeMark)-SI is a polyimide composed of two molar equivalents of dianhydrides: 4,4 -oxydiphthalic anhydride (ODPA), and 3,3 ,4,4 -biphenyltetracarboxylic dianhydride (BPDA) and 3,4 -oxydianiline (3,4 -ODA) as the diamine. The unique feature of this aromatic polyimide is that it remains soluble after solution imidization in high-boiling, polar aprotic solvents, even at solids contents of 50-percent by weight. However, once isolated and heated above its T(sub g) of 240 C, it becomes insoluble and exhibits high-temperature thermoplastic melt-flow behavior. With these unique structure property characteristics, it was thought this would be an advantage to have an aromatic polyimide that is both solution and melt processable in the imide form. This could potentially lead to lower cost production as it was not as equipment- or labor-intensive as other high-performance polyimide materials that either precipitate or are intractable. This unique combination of properties allowed patents with broad claim coverage and potential commercialization. After the U.S. Patent applications were filed, a Small Business Innovation Research (SBIR) contract was awarded to Imtec, Inc. to develop and supply the polyimide to NASA and the general public. Some examples of demonstration parts made with LARC(TradeMark)-SI ranged from aircraft wire and multilayer printed-circuit boards, to gears, composite panels, supported adhesive tape, composite coatings, cookware, and polyimide foam. Even with its unique processing characteristics, the thermal and mechanical properties were not drastically different from other solution or meltprocessable polyimides developed by NASA. LARC(TradeMark)-SI risked becoming another interesting, but costly, high-performance material.

Toxicity of pyrolysis gases from some cellular polymers

NASA Technical Reports Server (NTRS)

Hilado, C. J.; Machado, A. M.

1978-01-01

Various samples of cellular polymers were evaluated for toxicity of pyrolysis gases, using the screening test method developed at the University of San Francisco. The cellular polymer samples included polyimide, polymethacrylimide, polybismaleimide, polyurethane, polyisocyanurate, polyethylene, polychloroprene, polyvinyl chloride, polystyrene, polysiloxane, and polyphosphazene. The cellular polymers exhibited varying levels of toxicity under these test conditions. Among the rigid cellular polymers, times to death were shortest with the imide type foams and longest with polyvinyl chloride and polystyrene. Among the flexible cellular polymers, times to death were shortest with polyimide and polyester, and longest with polychloroprene and polysiloxane. Increased char yield was not necessarily associated with reduced toxicity.

Phenylethynyl amine

NASA Technical Reports Server (NTRS)

Hergenrother, Paul M. (Inventor); Bryant, Robert G. (Inventor); Jensen, Brian J. (Inventor); Havens, Stephen J. (Inventor)

1997-01-01

Four phenylethynyl amine compounds--3 and 4-aminophenoxy-4'-phenylethynylbenzophenone, and 3 and 4-amino-4'-phenylethynylbenzophenone--were readily prepared and were used to endcap imide oligomers. Phenylethynyl-terminated amide acid oligomers and phenylethynyl-terminated imide oligomers with various molecular weights and compositions were prepared and characterized. These oligomers were cured at 300.degree. C. to 400.degree. C. to provide crosslinked polyimides with excellent solvent resistance, high strength and modulus and good high temperature properties. Adhesive panels, composites, films and moldings from these phenylethynyl terminated imide oligomers gave excellent mechanical performance.

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.

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.

Synthesis and Characterization of Processable Polyimides with Enhanced Thermal Stability

NASA Technical Reports Server (NTRS)

Harris, Frank W.

1999-01-01

The following is a summary report of the research carried out under NASA Grant NAG-1-448. The work was divided into four major areas: 1) Enhanced polyimide processing through the use of reactive plasticizers 2) Development of processable polyhenylquinoxalines 3) Synthesis and characterization of perfluorovinylether-terminated imide oligomers and 4) Fluorosilicones containing perfuorocyclobutane rings.

Preparation and Characterization of Polyimide/Organoclay Nanocomposites

NASA Technical Reports Server (NTRS)

Delozier, D. M.; Orwoll, R. A.; Cahoon, J. F.; Johnston, N. J.; Smith, J. G., Jr.; Connell, J. W.

2002-01-01

Organically modified montmorrrillonite clay, containing a long chain aliphatic quarternary ammonium cation, was used to prepare polyimide/organoclay hybrids. Several approaches were examined in an attempt to achieve fully exfoliated nanocomposites. These included simple mixing of the clay in a pre-made high molecular weight poly(amide acid) solution; simple mixing followed by sonication of the organoclay/poly(amide acid) solutions; and the preparation of high molecular weight poly(amide acid)s in the presence of the organoclay dispersed in N-methyl-2-pyrrolidinone (NMP). The best results were obtained using the in-situ polymerization approach. The resulting nanocomposite films (both amide acid and imide), containing 3-8% by weight of organoclay, were characterized by differential scanning calorimetry (DSC), dynamic thermogravimetric analysis (TGA), transmission electron microscopy (TEM), X-ray diffraction (XRD), and thin film tensile properties. A significant degree of dispersion was observed in the nanocomposite films of the amide acid and the imide. After thermal treatment of amide acid films to effect imidization, in both air and nitrogen, the films were visually darker than control films without clay and the level of clay dispersion appeared to have decreased. In the latter case, the separation between the layers of the clay decreased to a spacing less than that present in the original organoclay. These observations suggest that thermal degradation of the aliphatic quarternary ammonium cation occurred likely during thermal treatment to effect imidization and solvent removal. These thermal degradation effects were less pronounced when thermal treatment was performed under nitrogen. The polyimide/organoclay hybrid films exhibited higher room temperature tensile moduli and lower strength and elongation to break than the control films.

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.

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.

Isomer effects on polyimide properties

NASA Technical Reports Server (NTRS)

Stump, B. L.

1978-01-01

Thermally stable polyimide polymers were prepared. Parameters explored include asymmetry of substitution, addition of alkyl substituents to an aromatic ring, and an increase in the number of aromatic rings present in the diamine monomer. It is shown that the use of an asymmetrical diamine in the preparation of a polyimide produces a polymer with a markedly lowered glass transition temperature. This is achieved with little or no sacrifice of thermal stability. An alternate approach taken was to prepare imide monomers which are capable of addition-type polymerization.

Synthesis and Characterization of Modified Phenylethynyl Terminated Polyimides

NASA Technical Reports Server (NTRS)

Chang, Alice C.

1998-01-01

As an ongoing effort to develop structural adhesives for high performance aerospace applications, recent work has focused on phenylethynyl terminated imide (PETI) oligomers. The work reported herein involves the synthesis and characterization of a series of phenylethynyl containing oligomers designated LARC (TM) MPEI (Modified Phenylethynyl Terminated Polyimide). These oligomers contain mixtures of linear, branched and star-shaped molecules. The fully imidized polymers exhibited minimum melt viscosity as low as 600 poise at 335 C. Ti/Ti lap shear specimens processed at 288 C under 15 psi showed tensile shear strength of approx. 6000 psi and 5200 psi at ambient and 350 F temperatures, respectively. The chemistry and properties of these new MPEIs are presented and compared to an optimized linear PETI, LaRC(Tm) -PETI-5.

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.

Catalysts for polyimide foams from aromatic isocyanates and aromatic dianhydrides. [flame retardant foams

NASA Technical Reports Server (NTRS)

Riccitiello, S. R.; Sawko, P. M.; Estrella, C. A. (Inventor)

1979-01-01

Polyimide foam products having greatly improved burn-through and flame-spread resistance are prepared by the reaction of aromatic polyisocyanates with aromatic dianhydrides in the presence of metallic salts of octoic acid. The salts, for example stannous octoate, ferric octoate and aluminum octoate, favor the formation of imide linkages at the expense of other possible reactions.

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).

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.

Isomer effects on polyimide properties

NASA Technical Reports Server (NTRS)

Stump, B. L.

1975-01-01

The effect of structure variation on the solubility and glass-transition temperature of polyimide polymers is investigated. The addition of alkyl substituents to an aromatic ring in the polymer molecule, the reduction in the number of imide rings per average polymer chain-length, and a variation in the symmetry of the polymer molecule are studied. The synthesis of key intermediates for the preparation of the monomers required in this investigation is reported along with progress made in the synthesis of polyimide-precursor amines that contain functional groups to allow for post-cure cross-linking.

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).

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.

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.

Poly(imide-siloxane) segmented copolymer structural adhesives prepared by bulk and solution thermal imidization

NASA Technical Reports Server (NTRS)

Bott, R. H.; Summers, J. D.; Arnold, C. A.; Blankenship, C. P., Jr.; Taylor, L. T.

1988-01-01

The improved properties that have been demonstrated through thermal solution imidization in the case of polyimides and poly(imide-siloxane) segmented copolymers suggests significant potential for application of these new materials. Specifically, the enhancement in solubility, moisture reduction, and processability observed through this solution technique is quite dramatic. Previous work has shown that the presence of low amounts of siloxane does not detract significantly from the lap shear strength of these materials to titanium in the case of bulk thermal imidization synthesis. In addition, the siloxane incorporation results in the added advantage of resistance to hot, wet environments. This added durability is presumably due to the hydrophobic siloxane segments preventing the uptake of water at the critical interphase between the adhesive and the adherend. This paper discusses the extension of this work to the solution imidization synthesis technique recently developed in our laboratory. Results dealing with the absolute bond strengths as well as durability and failure surface analysis will be presented.

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.

Mechanical and spectroscopic properties of metal-containing polyimides

NASA Technical Reports Server (NTRS)

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

1983-01-01

The incorporation of specific metal ions into polyimides is described. Detailed studies have included various compounds of copper, lithium, and palladium as dopants. Addition of the metal during polymerization or after formation of the polyamic acid precedes the thermal imidization step. With many dianhydride-diamine-dopant combinations high quality variously colored films are produced. Many metal doped films exhibit (1) improved high temperature adhesive properties, (2) increased electrical conductivity, (3) excellent thermal stability, (4) improved acid/base resistance, (5) increased modulus in flexible films and (6) excellent high temperature tensile strength. X-ray photo-electron spectroscopic study of these films suggests that many of the additives undergo chemical modification during thermal imidization. Palladium dopants appear to be partially reduced to the metallic state, while lithium and copper dopants are probably converted to their oxides. Ion etching experiments with Auger electron spectroscopy monitoring are discussed.

Mechanical and spectroscopic properties of metal containing polyimides

NASA Technical Reports Server (NTRS)

Taylor, L. T.; St. Clair, A. K.

1984-01-01

The incorporation of specific metal ions into polyimides is described. Detailed studies have included various compounds of copper, lithium, and palladium as dopants. Addition of the metal during polymermzation or after formation of the polyamic acid precedes the thermal imidization step. With many dianhydride-diamine-dopant combinations high quality variously colored films are produced. Many metal doped films exhibit (1) improved high temperature adhesive properties, (2) increased electrical conductivity, (3) excellent thermal stability, (4) improved acid/base resistance, (5) increased modulus in flexible films and (6) excellent high temperature tensile strength. X-ray photo-electron spectroscopic study of these films suggests that many of the additives undergo chemical modification during thermal imidization. Palladium dopants appear to be partially reduced to the metallic state, while lithium and copper dopants are probably converted to their oxides. Ion etching experiments with Auger electron spectroscopy monitoring are discussed.

An investigation into the injection molding of PMR-15 polyimide

NASA Technical Reports Server (NTRS)

Colaluca, M. A.

1984-01-01

The chemorheological behavior of the PRM-15 molding compounds were characterized, the range of suitable processing parameters for injection molding in a reciprocating screw injection molding machine was determined, and the effects of the injection molding processing parameters on the mechanical properties of molded PMR-15 parts were studied. The apparatus and procedures for measuring viscosity and for determining the physical response of the material during heating are described. Results show that capillary rheometry can be effectively used with thermosets if the equipment is designed to overcome some of the inherent problems of these materials. A uniform temperature was provided in the barrel by using a circulating hot oil system. Standard capillary rheometry methods can provide the dependence of thermoset apparent viscosity on shear rate, temperature, and time. Process conditions resulting in complete imidization should be carefully defined. Specification of controlled oven temperature is inadequate and can result in incomplete imidization. For completely imidized PMR-15 heat at 15 C/min melt flow without gas evolution occurs in the temperature range of 325 C to 400 C.

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

Branched Rod-Coil Polyimide-Poly(Alkylene Oxide) Copolymers and Electrolyte Compositions

NASA Technical Reports Server (NTRS)

Meador, Maryann B. (Inventor); Tigelaar, Dean M. (Inventor)

2014-01-01

Crosslinked polyimide-poly(alkylene oxide) copolymers capable of holding large volumes of liquid while maintaining good dimensional stability. Copolymers are derived at ambient temperatures from amine endcapped amic-acid oligomers subsequently imidized in solution at increased temperatures, followed by reaction with trifunctional compounds in the presence of various additives. Films of these copolymers hold over four times their weight at room temperature of liquids such as ionic liquids (RTIL) and/or carbonate solvents. These rod-coil polyimide copolymers are used to prepare polymeric electrolytes by adding to the copolymers various amounts of compounds such as ionic liquids (RTIL), lithium trifluoromethane-sulfonimide (LiTFSi) or other lithium salts, and alumina.

Copoly(Imide Siloxane) Abhesive Materials with Varied Siloxane Oligomer Length

NASA Technical Reports Server (NTRS)

Wohl, Christopher J.; Atkins, Brad M.; Belcher, Marcus A.; Connell, John W.

2010-01-01

Incorporation of PDMS moieties into a polyimide matrix lowered the surface energy resulting in enhanced adhesive interactions. Polyimide siloxane materials were generated using amine-terminated PDMS oligomers of different lengths to study changes in surface migration behavior, phase segregation, mechanical, thermal, and optical properties. These materials were characterized using contact angle goniometry, tensile testing, and differential scanning calorimetry. The surface migration behavior of the PDMS component depended upon the siloxane molecular weight as indicated by distinct relationships between PDMS chain length and advancing water contact angles. Similar correlations were observed for percent elongation values obtained from tensile testing, while the addition of PDMS reduced the modulus. High fidelity topographical modification via laser ablation patterning further reduced the polyimide siloxane surface energy. Initial particulate adhesion testing experiments demonstrated that polyimide siloxane materials exhibited greater abhesive interactions relative to their respective homopolyimides.

Polyimide Foams

NASA Technical Reports Server (NTRS)

Vazquez, Juan M. (Inventor); Cano, Roberto J. (Inventor); Jensen, Brian J. (Inventor); Weiser, Erik S. (Inventor)

2005-01-01

A fully imidized, solvent-free polyimide foam having excellent mechanical, acoustic, thermal, and flame resistant properties is produced. A first solution is provided, which includes one or more aromatic dianhydrides or derivatives of aromatic dianhydrides, and may include one or more aromatic diamines, dissolved in one or more polar solvents, along with an effective amount of one or more blowing agents. This first solution may also advantageously include effective amounts respectively of one or mores catalysts, one or more surfactants, and one or more fire retardants. A second solution is also provided which includes one or more isocyanates. The first and second solutions are rapidly and thoroughly mixed to produce an admixture, which is allowed to foam-in an open container, or in a closed mold-under ambient conditions to completion produce a foamed product. This foamed product is then cured by high frequency electromagnetic radiation, thermal energy, or a combination thereof. Alternatively, the process is adapted for spraying or extrusion.

Polyimide foams

NASA Technical Reports Server (NTRS)

Weiser, Erik S. (Inventor); Cano, Roberto J. (Inventor); Jensen, Brian J. (Inventor); Vazquez, Juan M. (Inventor)

2005-01-01

A fully imidized, solvent-free polyimide foam having excellent mechanical, acoustic, thermal, and flame resistant properties is produced. A first solution is provided, which includes one or more aromatic dianhydrides or derivatives of aromatic dianhydrides, and may include one or more aromatic diamines, dissolved in one or more polar solvents, along with an effective amount of one or more blowing agents. This first solution may also advantageously include effective amounts respectively of one or mores catalysts, one or more surfactants, and one or more fire retardants. A second solution is also provided which includes one or more isocyanates. The first and second solutions are rapidly and thoroughly mixed to produce an admixture, which is allowed to foam?in an open container, or in a closed mold?under ambient conditions to completion produce a foamed product. This foamed product is then cured by high frequency electromagnetic radiation, thermal energy, or a combination thereof. Alternatively, the process is adapted for spraying or extrusion.

Polyimide foams

NASA Technical Reports Server (NTRS)

Vazquez, Juan M. (Inventor); Cano, Roberto J. (Inventor); Weiser, Erik S. (Inventor); Jensen, Brian J. (Inventor)

2009-01-01

A fully imidized, solvent-free polyimide foam having excellent mechanical, acoustic, thermal, and flame resistant properties is produced. A first solution is provided, which includes one or more aromatic dianhydrides or derivatives of aromatic dianhydrides, and may include one or more aromatic diamines, dissolved in one or more polar solvents, along with an effective amount of one or more blowing agents. This first solution may also advantageously include effective amounts respectively of one or mores catalysts, one or more surfactants, and one or more fire retardants. A second solution is also provided which includes one or more isocyanates. The first and second solutions are rapidly and thoroughly mixed to produce an admixture, which is allowed to foam--in an open container, or in a closed mold--under ambient conditions to completion produce a foamed product. This foamed product is then cured by high frequency electromagnetic radiation, thermal energy, or a combination thereof. Alternatively, the process is adapted for spraying or extrusion.

Novel aminobenzyl and imidobenzyl benzenes

NASA Technical Reports Server (NTRS)

Bell, V. L.; Pratt, J. R.; Stump, B. L.

1976-01-01

Compounds are useful as intermediates for several classes of polymers. Amines can function as cross-linking agents for epoxide and urethane polymers, as well as intermediates for synthesis of thermally-stable addition-type polyimides. Imide derivatives can be obtained by reacting amines with certain monoanhydrides containing olefinic unsaturation.

Molecular orientation in aligned electrospun polyimide nanofibers by polarized FT-IR spectroscopy.

PubMed

Yang, Haoqi; Jiang, Shaohua; Fang, Hong; Hu, Xiaowu; Duan, Gaigai; Hou, Haoqing

2018-07-05

Quantitative explanation on the improved mechanical properties of aligned electrospun polyimide (PI) nanofibers as the increased imidization temperatures is highly required. In this work, polarized FT-IR spectroscopy is applied to solve this problem. Based on the polarized FT-IR spectroscopy and the molecular model in the fibers, the length of the repeat unit of PI molecule, the angle between the fiber axis and the symmetric stretching direction of carbonyl group on the imide ring, and the angle between the PI molecular axis and fiber axis are all investigated. The Mark-Howink equation is used to calculate the number-average molar mass of PI molecules. The orientation states of PI molecules in the electrospun nanofibers are studied from the number-average molar mass of PI molecules and the average fiber diameter. Quantitative analysis of the orientation factor of PI molecules in the electrospun nanofibers is performed by polarized FT-IR spectroscopy. Copyright © 2018 Elsevier B.V. All rights reserved.

Annealing of aromatic polyimide precursors

NASA Technical Reports Server (NTRS)

Wakelyn, N. T.

1975-01-01

A study has been made of the thermal behavior of polyimide precursors: an isomeric pair of crystals of the complex formed by p-phenylenediamine with the separated isomers of the di-isopropyl ester of pyromellitic acid. Specimens of this material were isothermally annealed in the temperature range 120 C to 170 C for periods of time up to 1 week. Although this temperature range is well below that customarily used for imidizations, the working hypothesis was that it would be more likely that a polymer embodying at least part of the precursor structure could be formed if the molecular motion was minimized to that actually required for the formation of the imide linkage. The progress of the annealing was followed by: infrared spectroscopy, differential thermal analysis, powder X-ray diffraction, and thermal gravimetric analysis. Single crystal X-ray analysis of the meta monomer yields a structure of chains of alternating acid and base and suggests that this monomer is amenable to polymerization with a minimum of geometrical disruption.

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).

N-15 NMR Spectroscopy as a Method for Comparing the Rates of Imidization of Several Diamines

NASA Technical Reports Server (NTRS)

Johnson, J. Christopher; Kuczmarski, Maria A.

2006-01-01

The relative rates of the conversion of amide-acid to imide was measured for a series or aromatic diamines that have been identified as potential replacements for 4,4'-methylene dianiline (MDA) in high-temperature polyimides and polymer composites. These rates were compared with the N-15 NMR resonances of the unreacted amines. The initial rates of imidization track with the difference in chemical shift between the amine nitrogens in MDA and those in the subject diamines. This comparison demonstrated that N-15 NMR spectroscopy is appropriate for the rapid screening of candidate diamines to determine their reactivity relative to MDA, and can serve to provide guidance to the process of creating the time-temperature profiles used in processing these materials into polymer matrix composites.

Films, Preimpregnated Tapes and Composites Made from Polyimide "Salt-Like" Solutions

NASA Technical Reports Server (NTRS)

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

2001-01-01

High quality films, preimpregnated tape (prepegs), and composites have been fabricated from polyimide precursor 'saltlike' solutions. These salt-like solutions have a low viscosity (5,000 to 10,000 cp) and a high solids content (50-65% by weight) and can be coated onto reinforcing fiber to produce prepegs with excellent tack and drape at 12-15% residual solvent (approximately 4-6% water from thermal imidization reaction). The processing of these types of prepegs significantly overcomes solvent removal problems and allows excellent fiber wet out. In addition, the physical characteristics of the polyimide precursor salt-like solutions permits processing into high-performance materials through the use of standard prepregging and composite fabrication equipment. The resultant composites are of high quality.

Isomeric oxydiphthalic anhydride polyimides

NASA Technical Reports Server (NTRS)

Gerber, Margaret K.; Pratt, J. Richard; Stclair, Terry L.

1988-01-01

Much of the polyimide research at Langley Research Center has focused on isomeric modification of the diamine component; polyimides having considerably improved processability and adhesion have resulted. The present structure-property study was designed to investigate how isomeric attachment of the three oxydiphthalic anhydride (ODPA) polyimides affects their properties. Each dianhydride, 3,4,3',4'-oxydiphthalic anhydride (4,4'-OPDA,I), 2,3,2',3'-oxydiphthalic anhydride (3,3'-ODPA,II), and 2,3,3',4'-oxydiphthalic anhydride (3,4'-OPDA,III), was reacted with p-phenylenediamine, 4,4'-oxydianiline, 3,3'-diaminodiphenylsulfone, 3,3'-diaminobenzophenone, and 4,4'-bis(3-aminophenoxy)benzophenone in DMAc. The inherent viscosities of the resulting poly(amic acids) were determined. Thermally imidized films were studied for their creasability and solubility, as well as by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and wide angle X-ray scattering (WAXS). A comparison of these properties will be made.

Oxygen plasma resistant phosphine oxide containing imide/arylene copolymers

NASA Technical Reports Server (NTRS)

Jensen, Brian J.

1993-01-01

A series of oxygen plasma resistant imide/arylene ether copolymers were prepared by reacting anhydride-terminated poly(amide acids) and amine-terminated polyarylene ethers containing phosphine oxide units. Inherent viscosities for these copolymers ranged from 0.42 to 0.80 dL/g. After curing, the resulting copolymers had glass transition temperatures ranging from 224 C to 228 C. Solution cast films of the block copolymers were tough and flexible with tensile strength, tensile moduli, and elongation at break up to 16.1 ksi, 439 ksi, and 23 percent, respectively at 25 C and 9.1 ksi, 308 ksi and 97 percent, respectively at 150 C. The copolymers show a significant improvement in resistance to oxygen plasma when compared to the commercial polyimide Kapton. The imide/arylene ether copolymers containing phosphine oxide units are suitable as coatings, films, adhesives, and composite matrices.

Synthesis of tin-containing polyimide films

NASA Technical Reports Server (NTRS)

Ezzell, S. A.; Taylor, L. T.

1984-01-01

A series of tin-containing polyimide films derived from either 3,3',4,4'-benzophenone tetracarboxylic acid dianhydride or pyromellitic dianhydride and 4,4'-oxydianiline have been synthesized and their electrical properties examined. Highest quality materials (i.e., homogeneous, smooth surface, flexible) with the best electrical properties were doped with either SnCl2.2H2O or (n-Bu)2SnCl2. In all cases, extensive reactivity of the tin dopant with water, air or polyamic acid during imidization is observed. Lowered electrical surface resistivities appear to be correlatable with the presence of surface tin oxide on the film surface.

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.

High aspect ratio patterning of photosensitive polyimide with low thermal expansion coefficient and low dielectric constant

NASA Astrophysics Data System (ADS)

Dick, Andrew R.; Bell, William K.; Luke, Brendan; Maines, Erin; Mueller, Brennen; Rawlings, Brandon; Kohl, Paul A.; Grant Willson, C.

2016-07-01

A photosensitive polyimide system based on amine catalyzed imidization of a precursor poly(amic ester) is described. The material is based on the meta ethyl ester of pyromellitic dianhydride and 2,2' bis(trifluoromethyl)benzidine. It acts as a negative tone resist when formulated with a photobase generator. The material exhibits a dielectric constant of 3.0 in the gigahertz range, a coefficient of thermal expansion of 6±2 ppm/K, and can be patterned to aspect ratios of >2 when formulated with a highly quantum efficient cinnamide type photobase generator.

Polymide gas separation membranes

DOEpatents

Ding, Yong; Bikson, Benjamin; Nelson, Joyce Katz

2004-09-14

Soluble polyamic acid salt (PAAS) precursors comprised of tertiary and quaternary amines, ammonium cations, sulfonium cations, or phosphonium cations, are prepared and fabricated into membranes that are subsequently imidized and converted into rigid-rod polyimide articles, such as membranes with desirable gas separation properties. A method of enhancing solubility of PAAS polymers in alcohols is also disclosed.

Fabrication of polyimide-based nanocomposites containing functionalized graphene oxide nanosheets by in-situ polymerization and their properties

NASA Astrophysics Data System (ADS)

Qian, Yong; Lan, Yanfei; Xu, Jianping; Ye, Fucheng; Dai, Shizhen

2014-09-01

In this study, a facile and effective strategy is proposed to fabricate polyimide (PI)-based nanocomposites containing functionalized graphene oxide (FGO) nanosheets by in-situ polymerization and thermal imidization. Highly dispersed CIGO which was firstly obtained by graphene oxide (GO) functionalized with cyclohexyl isocyanate (CI) exhibited excellent dispersibility and compatibility in polyamic acid (PAA, precursor of PI) matrix via in-situ polymerization. Then the CIGO sheets were partially thermally reduced efficiently to FGO during the thermal imidization process of PAA. The incorporation of FGO sheets significantly affected the macroscopic properties of the PI-based composites. A 56.5% increase in the tensile strength and a 43.8% improvement in the Young's modulus were achieved for 2.0 wt% FGO loading. Furthermore, the thermal stability and glass transition temperature (Tg) were improved by adding FGO. In addition, the hydrophobic behavior of the PI-FGO composite clearly improved because of the excellent hydrophobic properties of FGO. The success of this approach provides a good rational for developing high-performance polymer-based composite materials.

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

Das, Sadananda; Brown, Suree S.; Mayes, Richard T.

A new series of amidoxime-based polymer adsorbents were synthesized at the Oak Ridge National Laboratory (ORNL) by electron beam induced grafting of acrylonitrile and itaconic acid onto polyethylene fiber. Hydroxylamine derivatives of poly(acrylonitrile) (PAN) moiety are demonstrated to possess two kinds of functional groups: open-chain amidoxime and cyclic imide dioxime. The open-chain amidoxime is shown to convert to imide dioxime on heat treatment in the presence of an aprotic solvent, like dimethylsulfoxide (DMSO). The formation of amidoxime and imide dioxime was confirmed by 13-C CPMAS spectra. The adsorbents were evaluated for uranium adsorption efficiency at ORNL with simulated seawater spikedmore » with 8 ppm uranium and 5 gallon seawater in a batch reactor, and in flow-through columns with natural seawater at the Marine Science Laboratory (MSL) of Pacific Northwest National Laboratory (PNNL) at Sequim Bay, WA. The DMSO-heat-treated sorbents adsorbed uranium as high as 4.48 g-U/kg-ads. from seawater. Experimental evidence is presented that the poly(imide dioxime) is primarily responsible for enhanced uranium adsorption capacity from natural seawater. The conjugated system in the imide dioxime ligand possesses increased electron donation ability, which is believed to significantly enhance the uranyl coordination in seawater« less

Surface modification of polyimide gate insulators for solution-processed 2,7-didecyl[1]benzothieno[3,2-b][1]benzothiophene (C10-BTBT) thin-film transistors.

PubMed

Jang, Kwang-Suk; Kim, Won Soo; Won, Jong-Myung; Kim, Yun-Ho; Myung, Sung; Ka, Jae-Won; Kim, Jinsoo; Ahn, Taek; Yi, Mi Hye

2013-01-21

The surface property of a polyimide gate insulator was successfully modified with an n-octadecyl side-chain. Alkyl chain-grafted poly(amic acid), the polyimide precursor, was synthesized using the diamine comonomer with an alkyl side-chain. By adding a base catalyst to the poly(amic acid) coating solution, the imidization temperature of the spin-coated film could be reduced to 200 °C. The 350 nm-thick polyimide film had a dielectric constant of 3.3 at 10 kHz and a leakage current density of less than 8.7 × 10(-10) A cm(-2), while biased from 0 to 100 V. To investigate the potential of the alkyl chain-grafted polyimide film as a gate insulator for solution-processed organic thin-film transistors (TFTs), we fabricated C(10)-BTBT TFTs. C(10)-BTBT was deposited on the alkyl chain-grafted polyimide gate insulator by spin-coating, forming a well-ordered crystal structure. The field-effect mobility and the on/off current ratio of the TFT device were measured to be 0.20-0.56 cm(2) V(-1) s(-1) and >10(5), respectively.

Optically transparent/colorless polyimides

NASA Technical Reports Server (NTRS)

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

1985-01-01

Several series of linear aromatic polyimide films have been synthesized and characterized with the objective of obtaining maximum optical transparency. Two approaches have been used as part of this structure-property relationship study. The first approach is to vary the molecular structure so as to separate chromophoric centers and reduce electronic interactions between polymer chains to lower the intensity of color in the resulting polymer films. A second and concurrent approach is to perform polymerizations with highly purified monomers. Glass transition temperatures of thermally cured polyimide films are obtained by thermomechanical analysis and thermal decomposition temperatures are determined by thermogravimetric analysis. Transmittance UV-visible spectra of the polyimide films are compared to that of a commercial polyimide film. Fully imidized films are tested for solubility in common organic solvents. The more transparent films prepared in this study are evaluated for use on second-surface mirror thermal control coating systems. Lightly colored to colorless films are characterized by UV-visible spectroscopy before and after exposure to 300 equivalent solar hours UV irradiation and varying doses of 1 MeV electron irradiation. The effects of monomer purity, casting solvent and cure atmosphere on polyimide film transparency are also investigated.

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

Surface Evaluation by XPS of High Performance Foams After Exposure to Oxygen Plasma

NASA Technical Reports Server (NTRS)

Hampton, Michael D.

2001-01-01

This report will present the results of a study done during a 10-week summer faculty fellowship during the summer of 2001 working with Ms. Martha Williams of the Testbeds Group at Kennedy Space Center. The work was in a new area for this faculty and was both interesting and enjoyable. An imide is a compound in which nitrogen is bonded directly to an R group and to two other R groups through carbonyls. Polyimides have a number of properties that make them highly desirable materials for use on structures that are exposed to extreme conditions. They are strong, fire resistant, minimally outgasing, stable over a large temperature range, resistant to chemical attack, transparent to infrared and microwaves, and have a low density. One polyimide, solimide, commercially available as a foam, retains resiliency from -300 F to +500 F, is highly flame retardant, and decomposes with virtually no smoke or toxic byproduct formation. The density of this product is such that its use in place of fiberglass in the lower lobe of a 747 saves 400 lb. Shipboard applications have resulted in literally tons of weight reduction. While polyimide films have been used in structures to be placed in low earth orbit (LEO) for many years, polyimide foams have found only minimal application in this realm. NASA Langley Research Center has developed new technology that allows for the processing of new polyimide foams. The resulting increased availability of these materials, along with their highly desirable properties, has prompted a study to determine the suitability of these materials for use in structures to be placed in LEO.

Space Environmentally Stable Polyimides and Copolyimides

NASA Technical Reports Server (NTRS)

Watson, Kent A.; Connell, John W.

2000-01-01

Polyimides with a unique combination of properties including low color in thin films, atomic oxygen (AO), ultra-violet (UV) radiation resistance, solubility in organic solvents in the imide form, high glass transition (T(sub g)) temperatures and high thermal stability have been prepared and characterized. The polymers were prepared by reacting a novel aromatic diamine with aromatic dianhydrides in a polar aprotic solvent. The solubility of the polymers in the imide form as well as the color density of thin films were dependent upon the chemical structure of the dianhydride. Several thin films (25-50 mm thick) prepared by solution casting of amide acid or imide solutions exhibited very low color and high optical transparency (approximately 90%) as determined by UV/visible spectroscopy. The polymers exhibited T(sub g)s >200 C depending upon the structure of the dianhydride and temperatures of 5% weight loss approximately 500C in air as determined by dynamic thermogravimetric analysis. Thin films coated with silver/inconel were exposed to a high fluence of AO and 1000 equivalent solar hours of UV radiation. The effects of these exposures on optical properties were minor. These space environmentally durable polymers are potentially useful in a variety of applications on spacecraft such as thin film membranes on antennas, second-surface mirrors, thermal/optical coatings and multi-layer thermal insulation (MLI) blanket materials. The chemistry, physical and mechanical properties of the polymers as well as their responses to AO and UV exposure will be discussed.

Feasibility demonstration for electroplating ultra-thin polyimide film. [fabricating film for space erectable structures

NASA Technical Reports Server (NTRS)

Schneier, R.; Braswell, T. V.; Vaughn, R. W.

1978-01-01

The effect of electrodeposition variables on film thickness was investigated using a dilute polyimide solution as a bath into which aluminum (as foil or as a vapor deposited coating) was immersed. The electrodeposited film was dried for 2 hours at 93 C (primarily to remove solvent) and cured for 18 hours at 186 C. Infrared studies indicate that imide formation (curing) occurs at 149 C under vacuum. From a conceptual viewpoint, satisfactory film metallized on one side can be obtained by this method. The cured ultra thin polyimide film exhibits properties equivalent to those of commercial film, and the surface appearance of the strippable polyimide film compares favorably with that of a sample of commercial film of thicker gauge. The feasibility of manufacturing approximately one million sq m of ultra thin film capable of being joined to fabricate an 800 m by 9 800 m square from starting material 0.5 to 1 m wide for space erectable structures was demonstrated.

Colorless polyimide/organoclay nanocomposite substrates for flexible organic light-emitting devices.

PubMed

Kim, Jin-Hoe; Choi, Myeon-Chon; Kim, Hwajeong; Kim, Youngkyoo; Chang, Jin-Hae; Han, Mijeong; Kim, Il; Ha, Chang-Sik

2010-01-01

We report the preparation and application of indium tin oxide (ITO) coated fluorine-containing polyimide/organoclay nanocomposite substrate. Fluorine-containing polyimide/organoclay nanocomposite films were prepared through thermal imidization of poly(amic acid)/organoclay mixture films, whilst on which ITO thin films were coated on the films using a radio-frequency planar magnetron sputtering by varying the substrate temperature and the ITO thickness. Finally the ITO coated fluorine-containing polyimide/organoclay nanocomposite substrate was employed to make flexible organic light-emitting devices (OLED). Results showed that the lower sheet resistance was achieved when the substrate temperature was high and the ITO film was thick even though the optical transmittance was slightly lowered as the thickness increased. approximately 10 nm width ITO nanorods were found for all samples but the size of clusters with the nanorods was generally increased with the substrate temperature and the thickness. The flexible OLED made using the present substrate was quite stable even when the device was extremely bended.

Process for preparing an assembly of an article and a polyimide which resists dimensional change, delamination and debonding when exposed to changes in temperature

NASA Technical Reports Server (NTRS)

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

1994-01-01

An assembly of an article and a polyimide composition is prepared. The assembly resists dimensional change, delamination, or debonding when exposed to changes in temperature. An article is provided. A polyamic acid solution which yields a polyimide having a low coefficient of thermal expansion (CTE) was prepared. Equimolar quantities of an aromatic diamine and an aromatic dianhydride were reacted in a solvent medium to form a polyamic acid solution. A metal ion-containing additive was added to the solution. Examples of this additive are: TbCl3, DyCl3, ErCl3, TmCl3, Al(C5H7O2)3, and Er2S3. The polyamic acid solution was imidized and is combined with the article to form the assembly.

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.

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

Processable Polyimides Containing APB and Reactive End Caps

NASA Technical Reports Server (NTRS)

Jensen, Brian J.

2003-01-01

Imide copolymers that contain 1,3- bis(3-aminophenoxy)benzene (APB) and other diamines and dianhydrides and that are terminated with appropriate amounts of reactive end caps have been invented. The reactive end caps investigated thus far include 4-phenylethynyl phthalic anhydride (PEPA), 3- aminophenoxy-4-phenylethynylbenzop henone (3-APEB), maleic anhydride (MA), and 5-norbornene-2,3-dicarboxylic anhydride [also known as nadic anhydride (NA)]. The advantage of these copolyimides terminated with reactive groups, relative to other polyimides terminated with reactive groups, is a combination of (1) higher values of desired mechanical-property parameters and (2) greater ease of processing into useful parts.

Uniaxial Stretching of Poly(keto-ether-imide) Films

NASA Technical Reports Server (NTRS)

Hinkley, Jeffrey A.; Dezern, James F.; Feuz, L.; Klinedinst, D.

1999-01-01

Fully-cured aromatic polyimides were prepared from various combinations of five dianhydrides and six diamines. When heated progressively under constant load, most of the films elongated rapidly near their glass transition temperatures. In about half of the nineteen materials, the strain was self-limiting - a possible indication of strain-induced crystallinity. The presence of crystallinity was established unambiguously for one material.

Deposition and Characterization of Hermetic, Biocompatible Thin Film Coatings for Implantable, Electrically Active Devices

NASA Astrophysics Data System (ADS)

Sweitzer, Robyn K.

Retinal prostheses may be used to support patients suffering from Age-related macular degeneration or retinitis pigmentosa. A hermetic encapsulation of the poly(imide )-based prosthesis is important in order to prevent the leakage of water and ions into the electric circuitry embedded in the poly(imide) matrix. The deposition of amorphous aluminum oxide (by sputtering) and diamond like carbon (by pulsed laser ablation and vacuum arc vapor deposition) were studied for the application in retinal prostheses. The resulting thin films were characterized for composition, thickness, adhesion and smoothness by scanning electron microscopy-energy dispersive spectroscopy, atomic force microscopy, profilometry and light microscopy. Electrical stability was evaluated and found to be good. The as-deposited films prevented incursion of salinated fluids into the implant over two (2) three month trials soaking in normal saline at body temperature, Biocompatibility was tested in vivo by implanting coated specimen subretinally in the eye of Yucatan pigs. While amorphous aluminum oxide is more readily deposited with sufficient adhesion quality, biocompatibility studies showed a superior behavior of diamond-like carbon. Amorphous aluminum oxide had more adverse effects and caused more severe damage to the retinal tissue.

Polyimide aerogels cross-linked through amine functionalized polyoligomeric silsesquioxane.

PubMed

Guo, Haiquan; Meador, Mary Ann B; McCorkle, Linda; Quade, Derek J; Guo, Jiao; Hamilton, Bart; Cakmak, Miko; Sprowl, Guilherme

2011-02-01

We report the first synthesis of polyimide aerogels cross-linked through a polyhedral oligomeric silsesquioxane, octa(aminophenyl)silsesquioxane (OAPS). Gels formed from polyamic acid solutions of 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA), bisaniline-p-xylidene (BAX) and OAPS were chemically imidized and dried using supercritical CO(2) extraction to give aerogels having density around 0.1 g/cm(3). The aerogels are greater than 90 % porous, have high surface areas (230 to 280 m(2)/g) and low thermal conductivity (14 mW/m-K at room temperature). Notably, the polyimide aerogels cross-linked with OAPS have higher modulus than polymer reinforced silica aerogels of similar density and can be fabricated as both monoliths and thin films. Thin films of the aerogel are flexible and foldable making them an ideal insulation for space suits, and inflatable structures for habitats or decelerators for planetary re-entry, as well as more down to earth applications.

Optical properties of polyimides films treated by nanosecond pulsed electrical discharges in water

NASA Astrophysics Data System (ADS)

Sava, Ion; Kruth, Angela; Kolb, Juergen F.; Miron, Camelia

2018-01-01

Fluorinated polyimide films containing cobalt chloride based on hexafluoroisopropylidenediphthalic dianhydride and 4,4‧-diamino-3,3‧-dimethyl diphenylmethane were treated by nanosecond pulsed electrical discharges generated in distilled water. The polyimide films have been characterized by Fourier transform infrared (FTIR) spectra and contact angle measurements, optical transmission spectroscopy, and fluorescence spectroscopy. Significant changes in some intrinsic fluorescence features, such as the intensity and position of the emission peak, have been observed during exposure to water plasma. These effects have been considered to correlate with the development of specific chemical interactions between the liquid and the macromolecules, including the formation of hydrogen bridges. A slight increase in surface hydrophobicity was observed after plasma treatment. FTIR spectra showed a decrease in the intensity of the absorption band and an opening of the imide ring, depending on the treatment time.

Polyimide Aerogels Using Triisocyanate as Cross-linker.

PubMed

Nguyen, Baochau N; Meador, Mary Ann B; Scheiman, Daniel; McCorkle, Linda

2017-08-16

A family of polyimide (PI)-based aerogels is produced using Desmodur N3300A, an inexpensive triisocyanate, as the cross-linker. The aerogels are prepared by cross-linking amine end-capped polyimide oligomers with the triisocyanate. The polyimide oligomers are formulated using 2,2'-dimethylbenzidine, 4,4'-oxydianiline, or mixtures of both diamines, combined with 3,3',4,4'-biphenyltetracarboxylic dianhydride, and are chemically imidized at room temperature. Depending on the backbone chemistry, chain length, and polymer concentration, density of the aerogels ranged from 0.06 to 0.14 g/cm 3 and Brunauer-Emmett-Teller surface areas ranged from 350 to 600 m 2 /g. Compressive moduli of these aerogels were as high as 225 MPa, which are comparable to, or higher than, those previously reported prepared with similar backbone structures but with other cross-linkers. Because of their lower cost and commercial availability as cross-linker, the aerogels may have further potential as insulation for building and construction, clothing, sporting goods, and automotive applications, although lower-temperature stability may limit their use in some aerospace applications.

Poly(carbonate-imide) polymer

NASA Technical Reports Server (NTRS)

St. Clair, Terry L. (Inventor); Maudgal, Shubha (Inventor); Pratt, J. Richard (Inventor)

1987-01-01

A novel series of polymers and copolymers based on a polyimide backbone with the incorporation of carbonate moieties along the backbone. The process for preparing these polymers and copolymers is also disclosed as is a novel series of dinitrodiphenyl carbonates and diaminodiphenyl carbonates. The novel polymers and copolymers exhibit high temperature capability and because of the carbonate unit, many exhibit a high degree of order and/or crystallinity.

Adhesion and failure analysis of metal-polymer interface in flexible printed circuits boards

NASA Astrophysics Data System (ADS)

Park, Sanghee; Kim, Ye Chan; Choi, Kisuk; Chae, Heeyop; Suhr, Jonghwan; Nam, Jae-Do

2017-12-01

As device miniaturization in microelectronics is currently requested in the development of high performance device, which usually include highly-integrated metal-polyimide multilayer structures. A redistribution layer (RDL) process is currently emerging as one of the most advance fabrication techniques for on-chip interconnect and packaging. One of the major issues in this process is the poor adhesion of the metal-polyimide interfaces particularly in flexible circuit boards due to the flexibility and bendability of devices. In this study, low pressure O2 plasma treatment was investigated to improve the adhesion of metal-polyimide interfaces, using inductively coupled plasma (ICP) treatment. We identified that the adhesion of metal-polyimide interfaces was greatly improved by the surface roughness control providing 46.1 MPa of shear force in the ball shear test after O2 plasma treatment, compared 14.2 MPa without O2 plasma treatment. It was seemingly due to the fact that the adhesion in metal-polyimide interfaces was improved by a chemical conversion of C=O to C-O bonds and by a ring opening reaction of imide groups, which was confirmed with FT-IR analysis. In the finite element numerical analysis of metal-polyimide interfaces, the O2 plasma treated interface showed that the in-plane stress distribution and the vertical directional deformation agreed well with real failure modes in flexible circuits manufacturing.

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.

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.

Orbital transfer rocket engine technology program: Soft wear ring seal technology

NASA Technical Reports Server (NTRS)

Lariviere, Brian W.

1992-01-01

Liquid oxygen (LOX) compatibility tests, including autogenous ignition, promoted ignition, LOX impact tests, and friction and wear tests on different PV products were conducted for several polymer materials as verification for the implementation of soft wear ring seals in advanced rocket engine turbopumps. Thermoplastics, polyimide based materials, and polyimide-imide base materials were compared for oxygen compatibility, specific wear coefficient, wear debris production, and heat dissipation mechanisms. A thermal model was generated that simulated the frictional heating input and calculated the surface temperature and temperature distribution within the seal. The predictions were compared against measured values. Heat loads in the model were varied to better match the test data and determine the difference between the measured and the calculated coefficients of friction.

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

NASA Technical Reports Server (NTRS)

Wohl, Christoper J.; Atkins, Brad M.; Lin, Yi; Belcher, Marcus A.; Connell, John W.

2010-01-01

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

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.

Porous Cross-Linked Polyimide-Urea Networks

NASA Technical Reports Server (NTRS)

Meador, Mary Ann B. (Inventor); Nguyen, Baochau N. (Inventor)

2015-01-01

Porous cross-linked polyimide-urea networks are provided. The networks comprise a subunit comprising two anhydride end-capped polyamic acid oligomers in direct connection via a urea linkage. The oligomers (a) each comprise a repeating unit of a dianhydride and a diamine and a terminal anhydride group and (b) are formulated with 2 to 15 of the repeating units. The subunit was formed by reaction of the diamine and a diisocyanate to form a diamine-urea linkage-diamine group, followed by reaction of the diamine-urea linkage-diamine group with the dianhydride and the diamine to form the subunit. The subunit has been cross-linked via a cross-linking agent, comprising three or more amine groups, at a balanced stoichiometry of the amine groups to the terminal anhydride groups. The subunit has been chemically imidized to yield the porous cross-linked polyimide-urea network. Also provided are wet gels, aerogels, and thin films comprising the networks, and methods of making the networks.

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.

Thermosetting Poly(imide silsesquioxane)s Featuring Reduced Moisture Affinity and Improved Processability (Post-print)

DTIC Science & Technology

2013-09-11

regioisomerism provided a unique opportunity to study the effects of monomer architecture on properties . The type of isomer affects rheological and...cure characteristics but was found to have no discernible influence on cured state properties . The benefits of POSS co-oligomerization are 3-fold in...of monomer architecture on properties . The type of isomer affects rheological and cure characteristics but was found to have no discernible influence

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.

Environmentally stable polymers and coatings for space application: CH-5, supplement 10

NASA Technical Reports Server (NTRS)

Sykes, G.

1986-01-01

High molecular weight, randomly coupled poly(imide siloxane) soluble block copolymers were synthesized from bis(amino propyl) polydimethylsiloxane equilibrates of various molecular weights, aromatic metalinked diamines, and 3,3'-4,4'-benzophenone tetracarboxylic dianhydride (BTDA). Two synthetic procedures were successfully used to synthesize the poly(amic acid siloxane) intermediates. For both synthetic procedures, a cosolvent system was employed to achieve complete solvation of all components throughout the polymerization. Physical property characterization is continuing.

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.

Solid state polymerization and crystallography of polyimide precursors. Ph.D. Thesis - Va. Univ.

NASA Technical Reports Server (NTRS)

Wakelyn, N. T.

1974-01-01

Although the production of crystallinity in a polymeric system has historically led to commerically useful properties, the polyimides, prized for their high temperature characteristics, as customarily synthesized by melt or solution casting, are amorphous. It is shown that polymide containing residual crystallinity can be synthesized by isothermal annealing of crystals of the salt of the diisopropyl ester of pyromellitic acid and phenylene diamine. The reaction is topochemical in that the geometry of the polymer product is dependent upon that of the crystalline precursor. Infrared spectroscopy reveals the presence of imide absorption in the polymer, while powder diffractometry suggests residual crystallinity. Single crystal X-ray analysis of the monomer yields a structure of chains of alternating acid and base suggesting that the monomer is amenable to polymerization with a minimum of geometrical disruption.

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.

Cross-linked polyimides for integrated optics

NASA Astrophysics Data System (ADS)

Singer, Kenneth D.; Kowalczyk, Tony C.; Nguyen, Hung D.; Beuhler, Allyson J.; Wargowski, David A.

1997-01-01

We have investigated a promising class of polyimide materials for both passive and active electro-optic devices, namely crosslinkable polyimides. These fluorinated polyimides are soluble in the imidized form and are both thermally and photo-crosslinkable leading to easy processability into waveguide structures and the possibility of stable electro-optic properties. We have fabricated channel and slab waveguides and investigated the mechanism of optical propagation loss using photothermal deflection spectroscopy and waveguide loss spectroscopy, and found the losses to arise from residual absorption due to the formation of charge transfer states. The absorption is inhibited by fluorination leading to propagation losses as low as 0.3 dB/cm in the near infrared. Because of the ability to photocrosslink, channel waveguides are fabricated using a simple wet-etch process. Channel waveguides so formed are observed to have no excess loss over slab structures. Solubility followed by thermal cross-linking allows the formation of multilayer structures. We have produced electro-optic polymers by doping with the nonlinear optical chromophores, DCM and DADC; and a process of concurrent poling and thermal crosslinking. Multilayer structures have been investigated and poling fields optimized in the active layer by doping the cladding with an anti-static agent. The high glass-transition temperature and cross-linking leads to very stable electro-optic properties. We are currently building electro-optic modulators based on these materials. Progress and results in this area also are reported.

Polyimide Nanocomposites Prepared from High-Temperature, Reduced Charge Organoclays

NASA Technical Reports Server (NTRS)

Delozier, D. M.; Orwoll, R. A.; Cahoon, J. F.; Ladislaw, J. S.; Smith, J. G., Jr.; Connell, J. W.

2003-01-01

Montmorillonite clays modified with the dihydrochloride salt of 1,3-bis(3-aminophenoxy)benzene (APB) were used in the preparation of polyimide/organoclay hybrid films. Organoclays with varying surface charge based upon APB were prepared and examined for their dispersion behavior in the polymer matrix. High molecular weight poly(amide acid) solutions were prepared in the presence of the organoclays. Films were cast and subsequently heated to 300C to cause imidization. The resulting nanocomposite films, containing 3 wt% of organoclay, were characterized by transmission electron microscopy and X-ray diffraction. The clay's cation exchange capacity (CEC) played a key role in determining the extent of dispersion in the polyimide matrix. Considerable dispersion was observed in some of the nanocomposite films. The most effective organoclay was found to have a CEC of 0.70 meq/g. Nanocomposite films prepared with 3-8 wt% of this organoclay were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), and thin-film tensile testing. High levels of clay dispersion could be achieved even at the higher clay loadings. Results from mechanical testing revealed that while the moduli of the nanocomposites increased with increasing clay loadings, both strength and elongation decreased.

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.

Synthesis of improved moisture resistant polymers

NASA Technical Reports Server (NTRS)

Orell, M. K.

1979-01-01

The use of difluoromaleimide-capped prepolymers to provide improved moisture resistant polymers was investigated. Six different prepolymer formulations were prepared by two different methods. One method utilized the PMR approach to polyimides and the second method employed the normal condensation route to provide fully imidized prepolymers. Polymer specimens cured at 450 F exhibited adequate long-term stability in air at 400 F. Moisture absorption studies were conducted on one polymer formulation. Neat Polymer specimens exhibited weight gains of up to 2% (w/w) after exposure to 100% relative humidity at 344K (160 F) for 400 hours.

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.

Silver Nanowire Embedded Colorless Polyimide Heater for Wearable Chemical Sensors: Improved Reversible Reaction Kinetics of Optically Reduced Graphene Oxide.

PubMed

Choi, Seon-Jin; Kim, Sang-Joon; Jang, Ji-Soo; Lee, Ji-Hyun; Kim, Il-Doo

2016-09-14

Optically reduced graphene oxide (ORGO) sheets are successfully integrated on silver nanowire (Ag NW)-embedded transparent and flexible substrate. As a heating element, Ag NWs are embedded in a colorless polyimide (CPI) film by covering Ag NW networks using polyamic acid and subsequent imidization. Graphene oxide dispersed aqueous solution is drop-coated on the Ag NW-embedded CPI (Ag NW-CPI) film and directly irradiated by intense pulsed light to obtain ORGO sheets. The heat generation property of Ag NW-CPI film is investigated by applying DC voltage, which demonstrates unprecedentedly reliable and stable characteristics even in dynamic bending condition. To demonstrate the potential application in wearable chemical sensors, NO 2 sensing characteristic of ORGO is investigated with respect to the different heating temperature (22.7-71.7 °C) of Ag NW-CPI film. The result reveals that the ORGO sheets exhibit high sensitivity of 2.69% with reversible response/recovery sensing properties and minimal deviation of baseline resistance of around 1% toward NO 2 molecules when the temperature of Ag NW-CPI film is 71.7 °C. This work first demonstrates the improved reversible NO 2 sensing properties of ORGO sheets on flexible and transparent Ag NW-CPI film assisted by Ag NW heating networks. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Autogenous electrolyte, non-pyrolytically produced solid capacitor structure

DOEpatents

Sharp, Donald J.; Armstrong, Pamela S.; Panitz, Janda Kirk G.

1998-01-01

A solid electrolytic capacitor having a solid electrolyte comprising manganese dioxide dispersed in an aromatic polyamide capable of further cure to form polyimide linkages, the solid electrolyte being disposed between a first electrode made of valve metal covered by an anodic oxide film and a second electrode opposite the first electrode. The electrolyte autogenously produces water, oxygen, and hydroxyl groups which act as healing substances and is not itself produced pyrolytically. Reduction of the manganese dioxide and the water molecules released by formation of imide linkages result in substantially improved self-healing of anodic dielectric layer defects.

Autogenous electrolyte, non-pyrolytically produced solid capacitor structure

DOEpatents

Sharp, D.J.; Armstrong, P.S.; Panitz, J.K.G.

1998-03-17

A solid electrolytic capacitor is described having a solid electrolyte comprising manganese dioxide dispersed in an aromatic polyamide capable of further cure to form polyimide linkages, the solid electrolyte being disposed between a first electrode made of valve metal covered by an anodic oxide film and a second electrode opposite the first electrode. The electrolyte autogenously produces water, oxygen, and hydroxyl groups which act as healing substances and is not itself produced pyrolytically. Reduction of the manganese dioxide and the water molecules released by formation of imide linkages result in substantially improved self-healing of anodic dielectric layer defects. 2 figs.

Effects of alignment layer thickness on the pretilt angle of liquid crystals

NASA Astrophysics Data System (ADS)

Son, Jong-Ho; Zin, Wang-Cheol

2010-12-01

Mixture solutions of vertical- and planar-aligning polyimide precursors were coated on bare glass. The concentrations of the solutions were varied to control the thicknesses of the films. The resulting blend films were baked to induce imidization and then rubbed. The thicknesses (t) of the blend film and of the pure vertical-alignment film affected their surface energies; the pretilt angle can be fully controlled in the range 5.5°≤Θ0≤87° by adjusting t. The surface energy of pure planar-alignment layers was independent of t.

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.

Zr-Containing 4,4'-ODA/PMDA Polyimide Composites. Parts 1 & 2

NASA Technical Reports Server (NTRS)

Illingsworth, M. L.; Betancourt, J. A.; Chen, Y.; Terschak, J. A.; Banks, B. A.; Rutledge, S. K.; Cales, M.; He, L.

2001-01-01

The objective of this research is to improve the atomic oxygen resistance of Kapton(TM), a polyimide (PI) made from pyromellitic acid dianhydride (PMDA) and 4,4'-oxydianiline (ODA), while retaining or enhancing the desirable properties of the pure polymer. Toward this end, zirconium-containing complexes and polymers were used to make composites and blends. Tetra(acetylacetonato)zirconium(IV), Zr(acac)4, which is commercially available, was identified as the best zirconium-containing complex for enhancing the atomic oxygen resistance of polyimide composites of the 10 complexes screened. Films prepared from the commercially available polyamic acid (PAA) of PMDA-ODA (DuPont) have good uniformity, flexibility, and tensile strength. A 24-layer 10% (mol) Zr(acac)4/PI composite film showed significant improvement (ca. 20 fold) of atomic oxygen resistance over the pure polyimide. However, 10% (mol) Zr(acac)4 represents an upper concentration limit, above which films undergo cracking upon thermal imidization. In order to increase the Zr complex concentration in PMDA-ODA PI films, while retaining good film properties, [Zr(adsp)2-PMDA]n coordination polymer [bis(4-amino-N,N'-disalicylidene- 1,2-phenylenediamino)zirconium(IV)-pyromellitic dianhydride] and [Zr(adsp)2-PMDA-ODA-PMDA]n terpolymer were synthesized and blended with commercial PAA, respectively. Several techniques were used to characterize the films made from the polymer containing Zr(acac)4. Plasma studies of films having 2% (mol) incremental concentrations of Zr in the Kapton up to 10% (mol) show that the overall rate of erosion is reduced about 75 percent.

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.

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.

The crystallization and crystalline properties of LARC-TPI

NASA Technical Reports Server (NTRS)

Theil, Michael H.; Gangal, Pravin D.

1992-01-01

LARC-TPI, a thermoplastic polyimide, has been studied in order to develop an understanding of its crystalline phase transition. Our experiments suggest that samples synthesized in different laboratories apparently had different degrees of imidization and their thermal behaviors differed accordingly. When the most crystalline of these polyimides was studied in some detail, we found that it melted irreversibly in that once a sample was completely melted it would not recrystallize. A polymer that did not recrystallize displayed a glass transition, which increased in temperature upon subsequent cooling and reheating. Solubility experiments indicated that heating above the crystalline melting temperature led to network formation in the polymer, a conclusion that is consistent with other behavior just mentioned. Differential calorimetric studies revealed that annealing at slow heating rates or under isothermal conditions resulted in dual melting transitions. These studies, supported by X-ray diffraction results, strongly indicate that the annealing process involves a solid-liquid-solid transformation. From an existing phenomenological model for the kinetics of phase transitions, kinetic parameters for these crystallizations have been evaluated. The Avrami exponents n increased with the annealing temperature in the protocol used in this study. Their values were about 2 or lower, thus indicating that crystallization may have followed a mechanism that included heterogeneous nucleation of a low dimensional order in which all the embryonic crystallites formed at the beginning of the process. A positive temperature coefficient for these crystallizations indicated that diffusion may have had a rate controlling influence and affected the values of n.

Design, fabrication and test of graphite/polyimide composite joints and attachments for advanced aerospace vehicles

NASA Technical Reports Server (NTRS)

Barclay, D. L.

1980-01-01

Results of an experimental program to develop several types of graphite/polyimide (GR/PI) bonded and bolted joints for lightly loaded flight components for advanced space transportation systems and high speed aircraft are presented. Tasks accomplished include: a literature survey; design of static discriminator specimens; design allowables testing; fabrication of test panels and specimens; small specimen testing; and standard joint testing. Detail designs of static discriminator specimens for each of the four major attachment types are presented. Test results are given for the following: (1) transverse tension of Celion 3000/PMR-15 laminate; (2) net tension of a laminate for both a loaded and unloaded bolt hole; (3) comparative testing of bonded and co-cured doublers along with pull-off tests of single and double bonded angles; (4) single lap shear tests, transverse tension and coefficient of thermal expansion tests of A7F (LARC-13 amide-imide modified) adhesive; and (5) tension tests of standard single lap, double lap, and symmetric step lap bonded joints. Also, included are results of a finite element analysis of a single lap bonded composite joint.

Synthesis and Compatibility of Ionic Liquid Containing Rod-Coil Polyimide Gel Electrolytes with Lithium Metal Electrodes

NASA Technical Reports Server (NTRS)

Tigelaar, Dean M.; Palker, Allyson E.; Meador, Mary Ann B.; Bennett, William R.

2008-01-01

A highly cross-linked polyimide-polyethylene oxide copolymer has been synthesized that is capable of holding large volumes of liquid component, simultaneously maintaining good dimensional stability. An amine end capped oligomer was made that was imidized in solution, followed by reaction with a triisocyanate in the presence of desired additives at ambient temperature. Polymer films are able to hold over 4 times their weight in room temperature ionic liquid RTIL or carbonate solvent. Electrolytes were studied that contained varying amounts of RTIL, lithium trifluoromethanesulfonimide LiTFSi, and alumina nanoparticles. Electrochemical stability of these electrolytes with lithium metal electrodes was studied by galvanic cycling and impedance spectroscopy. Improved cycling stability and decreased interfacial resistance were observed when increasing amounts of RTIL and LiTFSi were added. The addition of small amounts of alumina further decreased interfacial resistance by nearly an order of magnitude. During the course of the study, cycling stability increased from less than 3 to greater than 1000 h at 60 C and 0.25 mA/cm2 current density.

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.

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.

Synthesis of improved moisture resistant polymers

NASA Technical Reports Server (NTRS)

Scola, D. A.; Pater, R. H.

1978-01-01

The synthesis and characterization of novel moisture resistant aliphatic polyimides are described. Several novel aliphatic imides of diversified functionalities were synthesized, purified, and characterized, they include: (1) N-(12-aminododecyl)-5-norbornene-2,3-dicarboximide; (2) N,N'-2,2,2-trifluoro-1-(trifluoromethyl)ethylidene bis (1,3-dioxo-5,2-iosoindolinediyl)dodecamethylene di-5-norbornene-2,3-dicarboximide; (3) N,N'-dodecamethylenedi-5-nobornene-2,3-dicarbonoximide; (4) N,N'-dodecamethylenebis 5,6-epoxy-2,3-norbornanedicarboximide ; and (5) N,N'-Bis 12-(5-norbornene-2, 3-dicarboximidido)dodecyl - 1,2,3,4- butanetetracarboxylic 1,2:3,4-diimide. The structures of these compounds were established by elemental analysis, IR, NMR, and mass spectra.

New monomers for high performance polymers

NASA Technical Reports Server (NTRS)

Gratz, Roy F.

1993-01-01

This laboratory has been concerned with the development of new polymeric materials with high thermo-oxidative stability for use in the aerospace and electronics industries. Currently, there is special emphasis on developing matrix resins and composites for the high speed civil transport (HSCT) program. This application requires polymers that have service lifetimes of 60,000 hr at 350 F (177 C) and that are readily processible into void-free composites, preferably by melt-flow or powder techniques that avoid the use of high boiling solvents. Recent work has focused on copolymers which have thermally stable imide groups separated by flexible arylene ether linkages, some with trifluoromethyl groups attached to the aromatic rings. The presence of trifluoromethyl groups in monomers and polymers often improves their solubility and processibility. The goal of this research was to synthesize several new monomers containing pendant trifluoromethyl groups and to incorporate these monomers into new imide/arylene ether copolymers. Initially, work was begun on the synthesis of three target compounds. The first two, 3,5-dihydroxybenzo trifluoride and 3-amino 5-hydroxybenzo trifluoride, are intermediates in the synthesis of more complex monomers. The third, 3,5-bis (3-amino-phenoxy) benzotrifluoride, is an interesting diamine that could be incorporated into a polyimide directly.

Polyimide Based Nanocomposites for Affordable Space Transport

NASA Technical Reports Server (NTRS)

Dean, Derrick; Islam, Mohsina; Small, Sharee; Aldridge, Brandon; Campbell, Sandra G. (Technical Monitor)

2001-01-01

In setting forth its strategic plan, NASA has indicated that low-cost access to space is the key to unleashing the commercial potential of space and greatly expanding space research and exploration. The development of advanced materials will be an enabling technology for this quest for low-cost space access. In this research program, we are attempting to address the need for new advanced materials by developing high-performance nanodispersed inorganic/organic and organic/organic polyimide composites utilizing specific interactions. Our goal is to systematically manipulate these interactions and investigate the resulting processing morphology-property relationships. Specifically, we will investigate three main parameters on these relationships. These include (1) the type of polyimide; (2) the structure of the inorganic nanoparticle being used; and (3) manipulation of the interfacial energy. During the first year of this effort, we have demonstrated the successful synthesis of PMR-15/layered silicate nanocomposites. Morphological studies indicate that exfoliated structures were obtained in most instances, with a mixture of exfoliated and intercalated structures being observed also. Significant enhancements of the onset of decomposition were obtained by varying the strength of the interaction between the nanoparticle and the polymer. Varying the amount of a specific nanoparticle also affected the decomposition temperatures. A slight catalytic effect of the nanoparticles on both the imidization and crosslinking reaction has been observed and will be presented. In addition, incorporation of the nanoparticles was found to increase the glass transition temperature and slightly broaden the breadth of this relaxation.

High-frequency electromagnetic properties of soft magnetic metal-polyimide hybrid thin films

NASA Astrophysics Data System (ADS)

Kim, Sang Woo; Yoon, Chong S.

2007-09-01

Although there are a lot of demands for suppression of unwanted high-frequency electromagnetic noise in highly integrated electronic devices such as mobile phones and notebook computers, electromagnetic thin films that effectively work in the high-frequency range have still been underdeveloped. Soft magnetic metal-polyimide (PI) hybrid films with high electrical resistivity were prepared by thermal imidization and selective oxidation between the metal alloy layer and polyamic acid (PAA) layer. Electromagnetic properties of the hybrid thin films in the radio-frequency range were characterized by using the microstrip line method and were correlated with their material parameters. Although anisotropy field of the CoFe/NiFe hybrid film was two times lower than that of the NiFe hybrid film, the saturation magnetization of the CoFe/NiFe hybrid film was three times higher than that of the NiFe hybrid film. The CoFe/NiFe hybrid film showed higher power loss in the frequency range of 3-6 GHz compared to the NiFe hybrid film. The high power loss of the CoFe/NiFe hybrid film was caused by high relative permeability and high ferromagnetic resonance (FMR) frequency due to high saturation magnetization.

Travelers with immune-mediated inflammatory diseases: are they different?

PubMed

Jaeger, Veronika K; Rüegg, Rolanda; Steffen, Robert; Hatz, Christoph; Bühler, Silja

2015-01-01

Patients with immune-mediated inflammatory diseases (IMIDs) increasingly benefit from improved health due to new therapeutic regimens allowing increasing numbers of such patients to travel overseas. This study aims to assess the proportion of IMID travelers seeking advice at the Travel Clinic of the University of Zurich, Switzerland, and to determine whether demographics, travel, and vaccination patterns differ between IMID- and non-IMID travelers. Pre-travel visits and differences between IMID- and non-IMID travelers were assessed; logistic regression was used to adjust for confounders. Among 22,584 travelers who visited the Zurich Travel Clinic in a 25-month period, 1.8% suffered from an IMID, with gastroenterological and rheumatic conditions being the most common; 34.2% were using immunosuppressive or immunomodulatory medication. The reasons for travel and the destinations did not differ between IMID- and non-IMID travelers, Thailand and India being the most common destinations. IMID travelers stayed less often for longer than 1 month abroad and traveled less frequently on a low budget. Inactivated vaccines were similarly administered to both groups, while live vaccines were given half as often to IMID travelers. The increasing numbers of IMID patients, many using immunosuppressive or immunomodulatory therapy, show similar travel patterns as non-IMID travelers. Thus, they are exposed to the same travel health risks, vaccine-preventable infections being one among them. Particularly, in view of the fact that live attenuated vaccines are less often administered to IMID patients more data are needed on the safety and immunogenicity of vaccines and on travel-specific risks to be able to offer evidence-based pre-travel health advice. © 2014 International Society of Travel Medicine.

Processing and Properties of Fiber Reinforced Polymeric Matrix Composites. Part 2; Processing Robustness of IM7/PETI Polyimide Composites

NASA Technical Reports Server (NTRS)

Hou, Tan-Hung

1996-01-01

The processability of a phenylethynyl terminated imide (PETI) resin matrix composite was investigated. Unidirectional prepregs were made by coating an N-methylpyrrolidone solution of the amide acid oligomer onto unsized IM7. Two batches of prepregs were used: one was made by NASA in-house, and the other was from an industrial source. The composite processing robustness was investigated with respect to the effect of B-staging conditions, the prepreg shelf life, and the optimal processing window. Rheological measurements indicated that PETI's processability was only slightly affected over a wide range of B-staging temperatures (from 250 C to 300 C). The open hole compression (OHC) strength values were statistically indistinguishable among specimens consolidated using various B-staging conditions. Prepreg rheology and OHC strengths were also found not to be affected by prolonged (i.e., up to 60 days) ambient storage. An optimal processing window was established using response surface methodology. It was found that IM7/PETI composite is more sensitive to the consolidation temperature than to the consolidation pressure. A good consolidation was achievable at 371 C/100 Psi, which yielded an OHC strength of 62 Ksi at room temperature. However, processability declined dramatically at temperatures below 350 C.

Novel Phenylethynyl Imide Silanes as Coupling Agents for Titanium Alloy

NASA Technical Reports Server (NTRS)

Park, C.; Lowther, S. E.; Smith, J. G., Jr.; Conell, J. W.; Hergenrother, P. M.; SaintClair, T. L.

2004-01-01

The durability of titanium (Ti) alloys bonded with high temperature adhesives such as polyimides has failed to attain the level of performance required for many applications. The problem to a large part is attributed to the instability of the surface treatment on the Ti substrate. Although Ti alloy adhesive specimens with surface treatments such as chromic acid anodization, Pasa-Jell, Turco, etc. have provided high initial mechanical properties, these properties have decreased as a function of aging at ambient temperature and faster, when aged at elevated temperatures or in a hot-wet environment. As part of the High Speed Civil Transport program where Ti honeycomb sandwich structure must perform for 60,000 hours at 177 C, work was directed to the development of environmentally safe, durable Ti alloy surface treatments.

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.

Commercialization of LARC(TradeMark)-SI Polyimide Technology

NASA Technical Reports Server (NTRS)

Bryant, Robert G.

2008-01-01

LARC(TradeMark)-SI, Langley Research Center-Soluble Imide, was developed in 1992. This new polyimide won a 1995 Research and Development 100 Award, with the first patent issuing in 1997 and subsequent issued patents in 1998 and 2000. Currently, this polymer has been successfully licensed by NASA, and has generated revenues in excess of 1.4 million dollars. This might seem insignificant in comparison to industrially developed technology, where the customer is understood, technologies that use a novel assembly of commercial off the shelf (COTS) components, or software patents and "method based" innovations that do not require any material beyond labor, as examples. However, consider that LARC(TradeMark)-SI competes in areas currently dominated by traditional materials at a cost disadvantage ($350/lb) and that the physical-mechanical properties of LARC(TradeMark)-SI are similar to other high performance polymers. Indeed the success of this particular polymer was due to many factors and many lessons learned to the point that the invention was the most important, but least significant part in the commercialization of this material. This brief paper outlines the significant factors that occurred to make this technology available for the public access and application development that led to the licensing success of this material.

Polyimide encapsulated lithium-rich cathode material for high voltage lithium-ion battery.

PubMed

Zhang, Jie; Lu, Qingwen; Fang, Jianhua; Wang, Jiulin; Yang, Jun; NuLi, Yanna

2014-10-22

Lithium-rich materials represented by xLi2MnO3·(1 - x)LiMO2 (M = Mn, Co, Ni) are attractive cathode materials for lithium-ion battery due to their high specific energy and low cost. However, some drawbacks of these materials such as poor cycle and rate capability remain to be addressed before applications. In this study, a thin polyimide (PI) layer is coated on the surface of Li1.2Ni0.13Mn0.54Co0.13O2 (LNMCO) by a polyamic acid (PAA) precursor with subsequently thermal imidization process. X-ray diffraction (XRD), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HR-TEM) results confirm the successful formation of a PI layer (∼3 nm) on the surface of LNMCO without destruction of its main structure. X-ray photoelectron spectroscopy (XPS) spectra show a slight shift of the Mn valence state from Mn(IV) to Mn(III) in the PI-LNMCO treated at 450 °C, elucidating that charge transfer takes place between the PI layer and LNMCO surface. Electrochemical performances of LNMCO including cyclic stability and rate capability are evidently improved by coating a PI nanolayer, which effectively separates the cathode material from the electrolyte and stabilizes their interface at high voltage.

Preparation and Properties of Nanocomposites from Pristine and Modified SWCNTs of Comparable Average Aspect Ratios

NASA Technical Reports Server (NTRS)

Smith, Joseph G.; Delozier, Donavon M.; Watson, Kent A.; Connell, John W.; Bekyarova, E.; Haddon, R.; Yu, A.

2008-01-01

Low color, flexible, space-durable polyimide films with inherent and robust electrical conductivity to dissipate electrostatic charge (ESC) have been under investigation as part of a materials development activity for future NASA space missions. The use of single-walled carbon nanotubes (SWCNTs) is one means to achieving this goal. Even though the concentration of SWCNTs needed to achieve ESC dissipation is typically low, it is dependent upon purity, size, dispersion, and functionalization. In this study, SWCNTs prepared by the electric arc discharge method were used to synthesize nanocomposites using the LaRC(TradeMark) CP2 backbone as the matrix. Pristine and functionalized SWCNTs were mixed with an alkoxysilane terminated amide acid of LaRC(TradeMark) CP2 and the soluble imide form of the polymer and the resultant nanocomposites evaluated for mechanical, thermal, and electrical properties. Due to the preparative conditions for the pristine and functionalized SWCNTs, the average aspect ratio for both was comparable. This permitted the assessment of SWCNT functionalization with respect to various interactions (e.g. van der Waals, hydrogen bonding, covalent bond formation, etc.) with the matrix and the macroscopic effects upon nanocomposite properties. The results of this study are described herein.

Preparation and properties of in situ amino-functionalized graphene oxide/polyimide composite films

NASA Astrophysics Data System (ADS)

Lu, Yunhua; Hao, Jican; Xiao, Guoyong; Chen, Lin; Wang, Tonghua; Hu, Zhizhi

2017-11-01

The pure light-colored and transparent polyimide (PI) film was prepared from aromatic dianhydride 4,4‧-(hexafluoroisopropylidene)diphthalic anhydride (6FDA) and diamine 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene (6FAPB) in the solvent of DMAc via two-step method. Graphene oxide (GO) was in situ grafted with 6FAPB and directly used as a functional inorganic nanofiller to further synthesize poly(amic acid) (PAA)/GO solution. Then, PI/GO composite films with different loadings of GO were prepared by the thermal imidization. The mechanical, thermal, optical, electrical, surface properties, and electrochemical behavior were characterized. The FTIR and XPS results indicate that amino groups can be successfully grafted on the surface of GO. The tensile strength and Young's modulus of the PI-1.0%GO composite film were increased to 118.4 MPa and 2.91 GPa, respectively, which was an approximate improvement of 30.8% and 39.9% compared with pure PI film. These PI/GO composites showed around 256 °C for the glass transition temperature, and around 535 °C for the 5% thermal decomposition temperature, respectively. However, the optical transmittance was significantly decreased from 81.5% (pure PI) to 0.8% (PI-1.0%GO). Besides, the electrical conductivity increased from 1.6 × 10-13 S/m (pure PI) to 2.5 × 10-9 S/m (PI-1.0%GO). Furthermore, when the incorporation of GO was 1.0 wt%, an obvious reduction from 1.08% (pure PI) to 0.65% in the water uptake was observed for the PI/GO composite films, and the water surface contact angle raised from 72.5° (pure PI) to 83.5°. The electrochemical behavior showed that the ability of oxygen atom on the imide ring to gain and loss electron was increased due to incorporation of GO. These results indicated that the strong interfacial interaction between GO and PAA as well as uniform dispersion of GO in PI matrix were benefit to improve the mechanical, thermal, electrical properties and so on. The in situ amino-functionalized approach provides a strategy for preparing high-performance PI-based composite materials.

Rodent repellents: Preparation and properties of thiouronium compounds and cyclic imides

USGS Publications Warehouse

Bellack, E.; DeWitt, J.B.

1954-01-01

Syntheses and bioassays of cyclic imides and thiouronium compounds were carried out as part of a search for materials capable of preventing rodent damage to packaged commodities. Previous studies had shown that repellent activity was associated with functional groups containing nitrogen and sulfur, and was enhanced by the presence of ionic linkages. Twenty-seven thiouronium compounds and 40 imides, including 1 0 compounds not described previously, were prepared for these tests. Ten imides and 26 thiouronium compounds were repellent under the conditions of test. Information obtained in these studies will be utilized in the development and selection of more effective materials for prevention of rodent damage to foods and other commodities.

Multidisciplinary Management of Spondyloarthritis-Related Immune-Mediated Inflammatory Disease.

PubMed

Rizzello, Fernando; Olivieri, Ignazio; Armuzzi, Alessandro; Ayala, Fabio; Bettoli, Vincenzo; Bianchi, Luca; Cimino, Luca; Costanzo, Antonio; Cristaudo, Antonio; D'Angelo, Salvatore; Daperno, Marco; Fostini, Anna Chiara; Galeazzi, Mauro; Gilio, Michele; Gionchetti, Paolo; Gisondi, Paolo; Lubrano, Ennio; Marchesoni, Antonio; Offidani, Annamaria; Orlando, Ambrogio; Pugliese, Daniela; Salvarani, Carlo; Scarpa, Raffaele; Vecchi, Maurizio; Girolomoni, Giampiero

2018-04-01

Immune-mediated inflammatory diseases (IMIDs) are chronic autoimmune conditions that share common pathophysiologic mechanisms. The optimal management of patients with IMIDs remains challenging because the coexistence of different conditions requires the intervention of several specialists. The aim of this study was to develop a series of statements defining overarching principles that guide the implementation of a multidisciplinary approach for the management of spondyloarthritis (SpA)-related IMIDs including SpA, psoriasis, psoriatic arthritis, Crohn's disease, ulcerative colitis and uveitis. A Delphi consensus-based approach was used to identify a core set of statements. The process included development of initial questions by a steering committee, an exhaustive search of the literature using complementary approaches to identify potential statements and two Delphi voting rounds for finalization of the statements. Consensus was achieved on the related nature of IMIDs, the existence of a high prevalence of multiple IMIDs in a single patient and the fact that a multidisciplinary approach can result in a more extensive evaluation and comprehensive approach to treatment. The goals of a multidisciplinary team should be to increase diagnosis of concomitant IMIDs, improve the decision-making process, and increase patient satisfaction and adherence. Early referral and diagnosis, early recognition of concomitant IMIDs and optimizing treatment to improve patient quality of life are some of the advantages of using multidisciplinary teams. To be effective, a multidisciplinary team should be equipped with the appropriate tools for diagnosis and follow-up, and at a minimum the multidisciplinary team should include a dermatologist, gastroenterologist and rheumatologist; providing psychologic support via a psychologist and involving an ophthalmologist, general practitioners and nurses in multidisciplinary care is also important. The present Delphi consensus identified a set of overarching principles that may be useful for implementation of a multidisciplinary approach for the management of SpA-related IMIDs. Aristea and Hippocrates.

Effect of interface structure regulation caused by variation of imidization rate on conduction current characteristics of PI/nano-Al2O3 three-layer composite films

NASA Astrophysics Data System (ADS)

Ma, Xinyu; Liu, Lizhu; Zhang, Xiaorui; He, Hongju

2018-06-01

A series of sandwich structure PI films were prepared by different imidization process, with pure PI film as the interlayer and PI/Al2O3 composite films as outer layers. The imidization rate of the film with different cured processes was calculated by characterizing by infrared spectrum (FT-IR), and the morphology of interlayer interface with different imidization rates by scanning electron microscope (SEM). When the imidization conditions of the first and second films were 260 °C/120 min, the composite films displayed better interface structure and higher imidization rate (ID) than others. Moreover, results also showed that the conduction current of three-layer composite film steadily improved with increased ID and temperature, and was higher than that of the pure film. At the temperature of 30 °C, the electrical aging threshold at different ID was obtained. When the ID reached the maximum value of 78.9%, the electrical aging threshold reached the maximum 41.69 kV/mm.

Porous Polyimide Membranes Prepared by Wet Phase Inversion for Use in Low Dielectric Applications

PubMed Central

Kim, Soohyun; Jang, Keon-Soo; Choi, Hee-Dok; Choi, Seung-Hoon; Kwon, Seong-Ji; Kim, Il-Doo; Lim, Jung Ah; Hong, Jae-Min

2013-01-01

A wet phase inversion process of polyamic acid (PAA) allowed fabrication of a porous membrane of polyimide (PI) with the combination of a low dielectric constant (1.7) and reasonable mechanical properties (Tensile strain: 8.04%, toughness: 3.4 MJ/m3, tensile stress: 39.17 MPa, and young modulus: 1.13 GPa), with further thermal imidization process of PAA. PAA was simply synthesized from purified pyromellitic dianhydride (PMDA) and 4,4-oxydianiline (ODA) in two different reaction solvents such as γ-butyrolactone (GBL) and N-methyl-2-pyrrolidinone (NMP), which produce Mw/PDI of 630,000/1.45 and 280,000/2.0, respectively. The porous PAA membrane was fabricated by the wet phase inversion process based on a solvent/non-solvent system via tailored composition between GBL and NMP. The porosity of PI, indicative of a low electric constant, decreased with increasing concentration of GBL, which was caused by sponge-like formation. However, due to interplay between the low electric constant (structural formation) and the mechanical properties, GBL was employed for further exploration, using toluene and acetone vs. DI-water as a coagulation media. Non-solvents influenced determination of the PAA membrane size and porosity. With this approach, insight into the interplay between dielectric properties and mechanical properties will inform a wide range of potential low-k material applications. PMID:23615465

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.

Method for the production of fabricated hollow microspheroids

DOEpatents

Wickramanayake, Shan; Luebke, David R.

2015-06-09

The method relates to the fabrication of a polymer microspheres comprised of an asymmetric layer surrounding a hollow interior. The fabricated hollow microsphere is generated from a nascent hollow microsphere comprised of an inner core of core fluid surrounded by a dope layer of polymer dope, where the thickness of the dope layer is at least 10% and less than 50% of the diameter of the inner core. The nascent hollow microsphere is exposed to a gaseous environment, generating a vitrified hollow microsphere, which is subsequently immersed in a coagulation bath. Solvent exchange produces a fabricated hollow microsphere comprised of a densified outer skin surrounding a macroporous inner layer, which surrounds a hollow interior. In an embodiment, the polymer is a polyimide or a polyamide-imide, and the non-solvent in the core fluid and the coagulation bath is water. The fabricated hollow microspheres are particularly suited as solvent supports for gas separation processes.

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.

Sympathetic Nerve Hyperactivity in the Spleen: Causal for Nonpathogenic-Driven Chronic Immune-Mediated Inflammatory Diseases (IMIDs)?

PubMed

Bellinger, Denise L; Lorton, Dianne

2018-04-13

Immune-Mediated Inflammatory Diseases (IMIDs) is a descriptive term coined for an eclectic group of diseases or conditions that share common inflammatory pathways, and for which there is no definitive etiology. IMIDs affect the elderly most severely, with many older individuals having two or more IMIDs. These diseases include, but are not limited to, type-1 diabetes, obesity, hypertension, chronic pulmonary disease, coronary heart disease, inflammatory bowel disease, and autoimmunity, such as rheumatoid arthritis (RA), Sjőgren's syndrome, systemic lupus erythematosus, psoriasis, psoriatic arthritis, and multiple sclerosis. These diseases are ostensibly unrelated mechanistically, but increase in frequency with age and share chronic systemic inflammation, implicating major roles for the spleen. Chronic systemic and regional inflammation underlies the disease manifestations of IMIDs. Regional inflammation and immune dysfunction promotes targeted end organ tissue damage, whereas systemic inflammation increases morbidity and mortality by affecting multiple organ systems. Chronic inflammation and skewed dysregulated cell-mediated immune responses drive many of these age-related medical disorders. IMIDs are commonly autoimmune-mediated or suspected to be autoimmune diseases. Another shared feature is dysregulation of the autonomic nervous system and hypothalamic pituitary adrenal (HPA) axis. Here, we focus on dysautonomia. In many IMIDs, dysautonomia manifests as an imbalance in activity/reactivity of the sympathetic and parasympathetic divisions of the autonomic nervous system (ANS). These major autonomic pathways are essential for allostasis of the immune system, and regulating inflammatory processes and innate and adaptive immunity. Pathology in ANS is a hallmark and causal feature of all IMIDs. Chronic systemic inflammation comorbid with stress pathway dysregulation implicate neural-immune cross-talk in the etiology and pathophysiology of IMIDs. Using a rodent model of inflammatory arthritis as an IMID model, we report disease-specific maladaptive changes in β₂-adrenergic receptor (AR) signaling from protein kinase A (PKA) to mitogen activated protein kinase (MAPK) pathways in the spleen. Beta₂-AR signal "shutdown" in the spleen and switching from PKA to G-coupled protein receptor kinase (GRK) pathways in lymph node cells drives inflammation and disease advancement. Based on these findings and the existing literature in other IMIDs, we present and discuss relevant literature that support the hypothesis that unresolvable immune stimulation from chronic inflammation leads to a maladaptive disease-inducing and perpetuating sympathetic response in an attempt to maintain allostasis. Since the role of sympathetic dysfunction in IMIDs is best studied in RA and rodent models of RA, this IMID is the primary one used to evaluate data relevant to our hypothesis. Here, we review the relevant literature and discuss sympathetic dysfunction as a significant contributor to the pathophysiology of IMIDs, and then discuss a novel target for treatment. Based on our findings in inflammatory arthritis and our understanding of common inflammatory process that are used by the immune system across all IMIDs, novel strategies to restore SNS homeostasis are expected to provide safe, cost-effective approaches to treat IMIDs, lower comorbidities, and increase longevity.

Gold-catalyzed synthesis of benzil derivatives and α-keto imides via oxidation of alkynes.

PubMed

Xu, Cheng-Fu; Xu, Mei; Jia, Yi-Xia; Li, Chuan-Ying

2011-03-18

An efficient process based on the gold-catalyzed redox reaction has been developed to oxidize 1,2-diarylacetylene or ynamide to 1,2-diaryldiketone or α-keto imide respectively. This process can tolerate a variety of functional groups and affords 1,2-dicarbonyl compounds in excellent yields under mild reaction conditions.

Processing Robustness for A Phenylethynyl Terminated Polyimide Composite

NASA Technical Reports Server (NTRS)

Hou, Tan-Hung

2004-01-01

The processability of a phenylethynyl terminated imide resin matrix (designated as PETI-5) composite is investigated. Unidirectional prepregs are made by coating an N-methylpyrrolidone solution of the amide acid oligomer (designated as PETAA-5/NMP) onto unsized IM7 fibers. Two batches of prepregs are used: one is made by NASA in-house, and the other is from an industrial source. The composite processing robustness is investigated with respect to the prepreg shelf life, the effect of B-staging conditions, and the optimal processing window. Prepreg rheology and open hole compression (OHC) strengths are found not to be affected by prolonged (i.e., up to 60 days) ambient storage. Rheological measurements indicate that the PETAA-5/NMP processability is only slightly affected over a wide range of B-stage temperatures from 250 deg C to 300 deg C. The OHC strength values are statistically indistinguishable among laminates consolidated using various B-staging conditions. An optimal processing window is established by means of the response surface methodology. IM7/PETAA-5/NMP prepreg is more sensitive to consolidation temperature than to pressure. A good consolidation is achievable at 371 deg C (700 deg F)/100 Psi, which yields an RT OHC strength of 62 Ksi. However, processability declines dramatically at temperatures below 350 deg C (662 deg F), as evidenced by the OHC strength values. The processability of the IM7/LARC(TM) PETI-5 prepreg was found to be robust.

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).

Influence of Polymer-Clay Interfacial Interactions on the Ignition Time of Polymer/Clay Nanocomposites

PubMed Central

Zope, Indraneel S.; Yu, Zhong-Zhen

2017-01-01

Metal ions present on smectite clay (montmorillonite) platelets have preferential reactivity towards peroxy/alkoxy groups during polyamide 6 (PA6) thermal decomposition. This changes the decomposition pathway and negatively affects the ignition response of PA6. To restrict these interfacial interactions, high-temperature-resistant polymers such as polyetherimide (PEI) and polyimide (PI) were used to coat clay layers. PEI was deposited on clay by solution-precipitation, whereas PI was deposited through a solution-imidization-precipitation technique before melt blending with PA6. The absence of polymer-clay interfacial interactions has resulted in a similar time-to-ignition of PA6/PEI-clay (133 s) and PA6/PI-clay (139 s) composites as neat PA6 (140 s). On the contrary, PA6 with conventional ammonium-based surfactant modified clay has showed a huge drop in time-to-ignition (81 s), as expected. The experimental evidences provided herein reveal the role of the catalytic activity of clay during the early stages of polymer decomposition. PMID:28800095

Influence of Polymer-Clay Interfacial Interactions on the Ignition Time of Polymer/Clay Nanocomposites.

PubMed

Zope, Indraneel S; Dasari, Aravind; Yu, Zhong-Zhen

2017-08-11

Metal ions present on smectite clay (montmorillonite) platelets have preferential reactivity towards peroxy/alkoxy groups during polyamide 6 (PA6) thermal decomposition. This changes the decomposition pathway and negatively affects the ignition response of PA6. To restrict these interfacial interactions, high-temperature-resistant polymers such as polyetherimide (PEI) and polyimide (PI) were used to coat clay layers. PEI was deposited on clay by solution-precipitation, whereas PI was deposited through a solution-imidization-precipitation technique before melt blending with PA6. The absence of polymer-clay interfacial interactions has resulted in a similar time-to-ignition of PA6/PEI-clay (133 s) and PA6/PI-clay (139 s) composites as neat PA6 (140 s). On the contrary, PA6 with conventional ammonium-based surfactant modified clay has showed a huge drop in time-to-ignition (81 s), as expected. The experimental evidences provided herein reveal the role of the catalytic activity of clay during the early stages of polymer decomposition.

Stretch-Oriented Polyimide Films

NASA Technical Reports Server (NTRS)

Hinkley, Jeffrey A.; Klinedinst, D.; Feuz, L.

2000-01-01

Two thermoplastic polyimides - one amorphous, the other crystallizable -- were subjected to isothermal stretching just above their glass transition temperatures. Room-temperature strengths in the stretch direction were greatly improved and, moduli increased up to 3.6-fold. Optimum stretching conditions were determined.

78 FR 57285 - 2,5-Furandione, Polymer With Ethenylbenzene, Hydrolyzed, 3-(Dimethylamino)propyl Imide, Imide...

Federal Register 2010, 2011, 2012, 2013, 2014

2013-09-18

..., Polymer With Ethenylbenzene, Hydrolyzed, 3- (Dimethylamino)propyl Imide, Imide With Polyethylene..., polymer with ethenylbenzene, hydrolyzed, 3-(dimethylamino)propyl imide, imide with polyethylene... to establish a maximum permissible level for residues of 2,5-furandione, polymer with ethenylbenzene...

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.

Room Temperature Halogenation of Polyimide Film Surface using Chlorine Trifluoride Gas

NASA Astrophysics Data System (ADS)

Habuka, Hitoshi; Kosuga, Takahiro; Koike, Kunihiko; Aida, Toshihiro; Takeuchi, Takashi; Aihara, Masahiko

2004-02-01

In order to develop a new application of chlorine trifluoride gas, the halogenation of a polyimide film surface at room temperature and at atmospheric pressure is studied for the first time. The polyimide film surface after exposure to the chlorine trifluoride gas shows a decreased water contact angle with increasing chlorine trifluoride gas concentration and exposure period. Since both X-ray photoelectron spectroscopy and infrared absorption spectroscopy simultaneously showed the formation of a carbon-chlorine bond and carbon-fluorine bond, it is concluded that the chlorine trifluoride gas can easily and safely perform the halogenation of the polyimide film surface under the stated conditions using a low-cost process and equipment.

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.

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.

Electrically Conductive Polyimide Films Containing Gold Surface

NASA Technical Reports Server (NTRS)

Caplan, Maggie L.; Stoakley, Diane M.; St. Clair, Anne K.

1994-01-01

Polyimide films exhibiting high thermo-oxidative stability and including electrically conductive surface layers containing gold made by casting process. Many variations of basic process conditions, ingredients, and sequence of operations possible, and not all resulting versions of process yield electrically conductive films. Gold-containing layer formed on film surface during cure. These metallic gold-containing polyimides used in film and coating applications requiring electrical conductivity, high reflectivity, exceptional thermal stability, and/or mechanical integrity. They also find commercial potential in areas ranging from thin films for satellite antennas to decorative coatings and packaging.

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.

Analyses of Failure Mechanisms and Residual Stresses in Graphite/Polyimide Composites Subjected to Shear Dominated Biaxial Loads

NASA Technical Reports Server (NTRS)

Kumosa, M.; Predecki, P. K.; Armentrout, D.; Benedikt, B.; Rupnowski, P.; Gentz, M.; Kumosa, L.; Sutter, J. K.

2002-01-01

This research contributes to the understanding of macro- and micro-failure mechanisms in woven fabric polyimide matrix composites based on medium and high modulus graphite fibers tested under biaxial, shear dominated stress conditions over a temperature range of -50 C to 315 C. The goal of this research is also to provide a testing methodology for determining residual stress distributions in unidirectional, cross/ply and fabric graphite/polyimide composites using the concept of embedded metallic inclusions and X-ray diffraction (XRD) measurements.

Targeting adequate thermal stability and fire safety in selecting ionic liquid-based electrolytes for energy storage.

PubMed

Chancelier, L; Diallo, A O; Santini, C C; Marlair, G; Gutel, T; Mailley, S; Len, C

2014-02-07

The energy storage market relating to lithium based systems regularly grows in size and expands in terms of a portfolio of energy and power demanding applications. Thus safety focused research must more than ever accompany related technological breakthroughs regarding performance of cells, resulting in intensive research on the chemistry and materials science to design more reliable batteries. Formulating electrolyte solutions with nonvolatile and hardly flammable ionic liquids instead of actual carbonate mixtures could be safer. However, few definitions of thermal stability of electrolytes based on ionic liquids have been reported in the case of abuse conditions (fire, shortcut, overcharge or overdischarge). This work investigates thermal stability up to combustion of 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide ([C1C4Im][NTf2]) and 1-butyl-1-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide ([PYR14][NTf2]) ionic liquids, and their corresponding electrolytes containing lithium bis(trifluoromethanesulfonyl)imide LiNTf2. Their possible routes of degradation during thermal abuse testings were investigated by thermodynamic studies under several experimental conditions. Their behaviours under fire were also tested, including the analysis of emitted compounds.

Production of polyimide ceria nanocomposites by development of molecular hook technology in nano-sonochemistry.

PubMed

Hatami, Mehdi

2018-06-01

Poly(amic acid), the precursor of polyimide (PI), was used for the preparation of PI/CeO 2 nanocomposites (NC)s by ultrasonic assisted technique via insertion of the surface modified CeO 2 nanoparticles (NP)s into PI matrix. In the preparation stages, in the first, the modifications of CeO 2 NPs by using hexadecyltrimethoxysilane (HDTMS) as a binder were targeted using ultrasonic waves. In the second step, newly designed PI structure was formed from the sonochemical imidization process as a molecular hook. In this step two different reactions were occurred. The acetic acid elimination reaction in the main chain of macromolecule, and the acetylation reaction in the side chains of poly(amic acid) were accomplished. By acetylation process the hook structure was created for trapping of the modified nanoparticles. In the final step the preparation of PI NCs were achieved by sonochemical process. The structural and thermal properties of pure PI and PI/CeO 2 NCs were studied by several techniques such as fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (NMR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), X-ray diffraction (XRD), and thermal analyses. FT-IR and 1 H NMR spectra confirmed the success in preparation of PI matrix. The FE-SEM, TEM, and AFM analyses showed the uniform distribution of CeO 2 NPs in PI matrix. The XRD patterns of NCs show the presence of crystalline CeO 2 NPs in amorphous PI matrix. The thermal analysis results reveal that, with increases in the content of CeO 2 NPs in PI matrix, the thermally stability factors of samples were improved. Copyright © 2018 Elsevier B.V. All rights reserved.

Electromagnetic interference shielding effectiveness of microcellular polyimide/in situ thermally reduced graphene oxide/carbon nanotubes nanocomposites

NASA Astrophysics Data System (ADS)

Yang, Hongli; Yu, Zhi; Wu, Peng; Zou, Huawei; Liu, Pengbo

2018-03-01

A simple and effective method was adopted to fabricate microcellular polyimide (PI)/reduced graphene oxide (GO)/multi-walled carbon nanotubes (MWCNTs) nanocomposites. Firstly, microcellular poly (amic acid) (PAA)/GO/MWCNTs nanocomposites were prepared through solvent evaporation induced phase separation. In this process, PAA and dibutyl phthalate (DBP) co-dissolved in N,N-dimethylacetamide (DMAc) underwent phase separation with DMAc evaporating, and DBP microdomains were formed in continuous PAA phase. Subsequently, PAA was thermally imidized and simultaneously GO was in situ reduced. After DBP was removed, the microcellular PI/reduced GO (RGO)/MWCNTs nanocomposites were finally obtained. When the initial filler loading was 8 wt%, the electrical conductivity of microcellular PI/RGO, PI/MWCNTs and PI/RGO/MWCNTs nanocomposites were 0.05, 0.02 and 1.87 S·m-1, respectively, and the electromagnetic interference (EMI) shielding efficiency (SE) of microcellular PI/RGO, PI/MWCNTs and PI/RGO/MWCNTs nanocomposites were 13.7-15.1, 13.0-14.3 and 16.6-18.2 dB, respectively. The synergistic effect between RGO and MWCNTs enhanced both the electrical conductivity and EMI shielding performance of the microcellular PI/RGO/MWCNTs nanocomposites. The dominating EMI shielding mechanism for these materials was microwave absorption. While the initial loading of GO and MWCNT was 8 wt%, the microcellular PI/RGO/MWCNTs nanocomposite (500 μm thickness) had extremely high specific EMI SE value of 755-823 dB·cm2·g-1. Its thermal stability was also obviously improved, the 5% weight loss temperature in nitrogen was 548 °C. In addition, it also possessed a high Young's modulus of 789 MPa.

Concentration and mobility of charge carriers in thin polymers at high temperature determined by electrode polarization modeling

NASA Astrophysics Data System (ADS)

Diaham, Sombel; Locatelli, Marie-Laure

2012-07-01

Charge carrier concentration (n0) and effective mobility (μeff) are reported in two polymer films (<10 μm) and in a very high temperature range (from 200 to 400 °C). This was possible thanks to an electrode polarization modeling of broadband dielectric spectroscopy data. It is shown that the glass transition temperature (Tg) occurrence has a strong influence on the temperature dependence of n0 and μeff. We carry out that n0 presents two distinct Arrhenius-like behaviors below and above Tg, while μeff exhibits a Vogel-Fulcher-Tamman behavior only above Tg whatever the polymer under study. For polyimide films, n0 varies from 1 × 1014 to 4 × 1016 cm-3 and μeff from 1 × 10-8 to 2 × 10-6 cm2 V-1 s-1 between 200 °C to 400 °C. Poly(amide-imide) films show n0 values between 6 × 1016 and 4 × 1018 cm-3 from 270 °C to 400 °C, while μeff varies between 1 × 10-10 and 2 × 10-7 cm2 V-1 s-1. Considering the activation energies of these physical parameters in the temperature range of investigation, n0 and μeff values appear as coherent with those reported in the literature at lower temperature (<80 °C). Surface charge carrier concentrations (nS) are reported and discussed for potential passivation (i.e., surface electrical insulation) applications. Polyimide films appear as good candidates due to nS values less than 1011 cm-2 up to 300 °C.

Comparison of the tribological properties at 25 C of seven different polyimide films bonded to 301 stainless steel

NASA Technical Reports Server (NTRS)

Fusaro, R. L.

1980-01-01

A pin-on-disk type of friction and wear apparatus was used to study the tribological properties of seven different polyimide films bonded to AISI 301 stainless steel disks at 25 C. It was found that the substrate material was extremely influential in determining the lubricating ability of the polyimide films. All seven films spalled in less than 1000 cycles of sliding. This was believed to be caused by poor adherence to the 301 stainless steel or the inability of the films to withstand the high localized tensile stresses imparted by the deformation of the soft substrate under sliding conditions. The friction coefficients obtained for six of the polyimides varied between 0.21 to 0.32 while one varied between 0.32 to 0.39.

PMR polyimide prepreg with improved tack characteristics

NASA Technical Reports Server (NTRS)

Serafini, T. T.; Delvigs, P.

1976-01-01

Current PMR Polyimide prepreg technology utilizes methanol or ethanol solvents for preparation of the PMR prepreg solutions. The volatility of these solvents limits the tack and drape retention characteristics of unprotected prepreg exposed to ambient conditions. Studies conducted to achieve PMR 15 Polyimide prepreg with improved tack and drape characteristics were described. Improved tack and drape retention were obtained by incorporation of an additional monomer. The effects of various levels of the added monomer on the thermo-oxidative stability and mechanical properties of graphite fiber reinforced PMR 15 composites exposed and tested at 316 C (600 F) were discussed.

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.

Simulation of space radiation effects on polyimide film materials for high temperature applications

NASA Technical Reports Server (NTRS)

Fogdall, L. B.; Cannaday, S. S.

1977-01-01

Space environment effects on candidate materials for the solar sail film are determined. Polymers, including metallized polyimides that might be suitable solar radiation receivers, were exposed to combined proton and solar electromagnetic radiation. Each test sample was weighted, to simulate the tension on the polymer when it is stretched into near-planar shape while receiving solar radiation. Exposure rates up to 16 times that expected in Earth orbit were employed, to simulate near-sun solar sailing conditions. Sample appearance, elongation, and shrinkage were monitored, noted, and documented in situ. Thermosetting polyimides showed less degradation or visual change in appearance than thermoplastics.

PMR Polyimide prepreg with improved tack characteristics. [Polymerization of Monomer Reactants applications to fiber reinforced plastics

NASA Technical Reports Server (NTRS)

Serafini, T. T.; Delvigs, P.

1978-01-01

Current PMR Polyimide prepreg technology utilizes methanol or ethanol solvents for preparation of the PMR prepreg solutions. The volatility of these solvents limits the tack and drape retention characteristics of unprotected prepreg exposed to ambient conditions. Studies conducted to achieve PMR 15 Polyimide prepreg with improved tack and drape characteristics are described. Improved tack and drape retention were obtained by incorporation of an additional monomer. The effects of various levels of the added monomer on the thermo-oxidative stability and mechanical properties of graphite fiber reinforced PMR 15 composites exposed and tested at 316 C (600 F) are discussed.

Method to Prepare Processable Polyimides with Non-Reactive Endgroups Using 1,3-bis(3-Aminophenoxy) Benzene

NASA Technical Reports Server (NTRS)

Jensen, Brian J. (Inventor)

2000-01-01

Polyimide copolymers were obtained containing 1,3-bis(3-aminophenoxy)benzene (APB) and other diamines and dianhydrides and terminating with the appropriate amount of a non-reactive endcapper, such as phthalic anhydride. Homopolymers containing only other diamines and dianhydrides which are not processable under conditions described previously can be made processable by incorporating various amounts of APB, depending on the chemical structures of the diamines and dianhydrides used. Polyimides that are more rigid in nature require more APB to impart processability than polyimides that are less rigid in nature. The copolymers that result from using APB to enhance processability have a unique combination of properties including excellent thin film properties, low pressure processing (200 psi and below), improved toughness, improved solvent resistance, improved adhesive properties, improved composite mechanical properties, long term melt stability (several hours at 390 C), and lower melt viscosities.

Method To Prepare Processable Polyimides With Reactive Endogroups Using 1,3-bis(3-aminophenoxy)benzene

NASA Technical Reports Server (NTRS)

Jensen, Brian J. (Inventor)

2001-01-01

Polyimide copolymers were obtained containing 1,3-bis(3-aminophenoxy)benzene (APB) and other diamines and dianhydrides and terminating with the appropriate amount of a non-reactive endcapper, such as phthalic anhydride. Homopolymers containing only other diamines and dianhydrides which are not processable under conditions described previously can be made processable by incorporating various amounts of APB, depending on the chemical structures of the diamines and dianhydrides used. Polyimides that are more rigid in nature require more APB to impart processability than polyimides that are less rigid in nature. The copolymers that result from using APB to enhance processability have a unique combination of properties including excellent thin film properties, low pressure processing (200 psi and below), improved toughness, improved solvent resistance, improved adhesive properties, improved composite mechanical properties, long term melt stability (several hours at 390 C), and lower melt viscosities.

Platinum(II) diimine complexes with catecholate ligands bearing imide electron-acceptor groups: synthesis, crystal structures, (spectro)electrochemical and EPR studies, and electronic structure.

PubMed

Shavaleev, Nail M; Davies, E Stephen; Adams, Harry; Best, Jonathan; Weinstein, Julia A

2008-03-03

A series of catechols with attached imide functionality (imide = phthalimide PHT, 1,8-naphthalimide NAP, 1,4,5,8-naphthalenediimide NDI, and NAP-NDI) has been synthesized and coordinated to the Pt (II)(bpy*) moiety, yielding Pt(bpy*)(cat-imide) complexes (bpy* = 4,4'-di- tert-butyl-2,2'-bipyridine). X-ray crystal structures of PHT and NAP complexes show a distorted square-planar arrangement of ligands around the Pt center. Both complexes form "head-to-tail" dimers in the solid state through remarkably short unsupported Pt...Pt contacts of 3.208 (PHT) and 3.378 A (NAP). The Pt(bpy*)(cat-imide) complexes are shown to combine optical (absorption) and electrochemical properties of the catecholate (electron-donor) and imide (electron-acceptor) groups. The complexes show a series of reversible reduction processes in the range from -0.5 to -1.9 V vs Fc (+)/Fc, which are centered on either bpy* or imide groups, and a reversible oxidation process at +0.07 to +0.14 V, which is centered on the catecholate moiety. A combination of UV-vis absorption spectroscopy, cyclic voltammetry, UV-vis spectroelectrochemistry, and EPR spectroscopy has allowed assignment of the nature of frontier orbitals in Pt(bpy*)(cat-imide) complexes. The HOMO in Pt(bpy*)(cat-imide) is centered on the catechol ligand, while the LUMO is localized either on bpy* or on the imide group, depending on the nature of the imide group involved. Despite the variations in the nature of the LUMO, the lowest-detectable electronic transition in all Pt(bpy*)(cat-imide) complexes has predominantly ligand-to-ligand (catechol-to-diimine) charge-transfer nature (LLCT) and involves a bpy*-based unoccupied molecular orbital in all cases. The LLCT transition in all Pt(bpy*)(cat-imide) complexes appears at 530 nm in CH2Cl2 and is strongly negatively solvatochromic. The energy of this transition is remarkably insensitive to the imide group present, indicating lack of electronic communication between the imide and the catechol moieties within the cat-imide ligand. The high extinction coefficient, approximately 6 x 10(3) L mol(-1) cm(-1) of this predominantly LLCT transition is the result of the Pt orbital contribution, as revealed by EPR spectroscopy of the complexes in various redox states. The CV profile of the oxidation process of Pt(bpy*)(cat-imide) in CH2Cl2 and DMF is concentration dependent, as was shown for NDI and PHT complexes as typical examples. Oxidation appears as a simple diffusion-limited process at low concentrations, with an increasing anodic-to-cathodic peak separation eventually resolving as two independent consecutive waves as the concentration of the complex increases. It is suggested that aggregation of the complexes in the diffusion layer in the course of oxidation is responsible for the observed concentration dependence. Overall, the Pt(bpy*)(cat-imide) complexes are electrochromic compounds in which a series of stepwise reversible redox processes in the potential range from 0.2 to -2 V (vs Fc (+)/Fc) leads to tuneable absorbencies between 300 and 850 nm.

Development and testing of improved polyimide actuator rod seals at higher temperatures for use in advanced aircraft hydraulic systems

NASA Technical Reports Server (NTRS)

Robinson, E. D.; Waterman, A. W.; Nelson, W. G.

1972-01-01

Polyimide second stage rod seals were evaluated to determine their suitability for application in advanced aircraft systems. The configurations of the seals are described. The conditions of the life cycle tests are provided. It was determined that external rod seal leakage was within prescribed limits and that the seals showed no signs of structural degradation.

Synthesis and characterization of a melt processable polyimide

NASA Technical Reports Server (NTRS)

Burks, H. D.; St.clair, T. L.

1982-01-01

A melt processable polyimide which contains sulfur and oxygen bridges between the aromatic rings (BDSDA/APB) was synthesized and characterized. Its physical, mechanical, thermal and flow properties were determined as was its resistance to some of the more commonly used solvents. The melt flow properties were measured for the temperature range 250 C - 350 C and under the conditions (stress/strain) encountered in commercial processes.

Evaluating the impact of two training interventions to improve diagnosis and case-management of malaria and pneumonia in Uganda.

PubMed

Ssebuliba, D M; Ouifki, R; Pretorius, C; Burnett, S M; Mbonye, M K; Naikoba, S; Willis, K; Weaver, M R

2017-01-01

We present an age-structured mathematical model of malaria and pneumonia to study the effect of two capacity-building interventions: Integrated Management of Infectious Diseases (IMID) and On-site Support Services (OSS). IMID leads to a reduction in malaria prevalence by more than 2·4% across the [0,5), [5,14) and [14,50) age groups. IMID + OSS reduces it by more than 16·0% across all age groups. IMID decreases pneumonia prevalence by more than 3·0% across all age groups while IMID + OSS decreases it by more than 1·0% across all age groups. The number of malaria and pneumonia deaths is reduced by 7·8% by IMID across all age groups and IMID + OSS decreases this number by 30·5% across all age groups, which translates to saving a life of a child per month. Prevalence of malaria-pneumonia for the [0,5) age group is 0·52% at baseline, and IMID and IMID + OSS reduce it by 6·6% and 23·6%, respectively. There is no change in incidence of malaria or pneumonia disease episodes. The results also indicate that triaging of children contributes more than 50% to the effect of the interventions in reduction of deaths and a range of 14-91% in reduction of disease cases.

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

NASA Technical Reports Server (NTRS)

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

2003-01-01

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

21 CFR 177.2450 - Polyamide-imide resins.

Code of Federal Regulations, 2013 CFR

2013-04-01

...) For the purpose of this section the polyamide-imide resins are derived from the condensation reaction...) The polyamide-imide resins (CAS Reg. No. 31957-38-7) derived from the condensation reaction of...

21 CFR 177.2450 - Polyamide-imide resins.

Code of Federal Regulations, 2012 CFR

2012-04-01

...) For the purpose of this section the polyamide-imide resins are derived from the condensation reaction...) The polyamide-imide resins (CAS Reg. No. 31957-38-7) derived from the condensation reaction of...

A Mild, Ferrocene-Catalyzed C–H Imidation of (Hetero)Arenes

PubMed Central

2015-01-01

A simple method for direct C–H imidation is reported using a new perester-based self-immolating reagent and a base-metal catalyst. The succinimide products obtained can be easily deprotected in situ (if desired) to reveal the corresponding anilines directly. The scope of the reaction is broad, the conditions are extremely mild, and the reaction is tolerant of oxidizable and acid-labile functionality, multiple heteroatoms, and aryl iodides. Mechanistic studies indicate that ferrocene (Cp2Fe) plays the role of an electron shuttle in the decomposition of the perester reagent, delivering a succinimidyl radical ready to add to an aromatic system. PMID:24654983

Mechanism of immunomodulatory drugs' action in the treatment of multiple myeloma

PubMed Central

Chang, Xiubao; Zhu, Yuanxiao; Shi, Changxin; Stewart, A. Keith

2014-01-01

Although immunomodulatory drugs (IMiDs), such as thalidomide, lenalidomide, and pomalidomide, are widely used in the treatment of multiple myeloma (MM), the molecular mechanism of IMiDs' action is largely unknown. In this review, we will summarize recent advances in the application of IMiDs in MM cancer treatment as well as their effects on immunomodulatory activities, anti-angiogenic activities, intervention of cell surface adhesion molecules between myeloma cells and bone marrow stromal cells, anti-inflammatory activities, anti-proliferation, pro-apoptotic effects, cell cycle arrest, and inhibition of cell migration and metastasis. In addition, the potential IMiDs' target protein, IMiDs' target protein's functional role, and the potential molecular mechanisms of IMiDs resistance will be discussed. We wish, by presentation of our naive discussion, that this review article will facilitate further investigation in these fields. PMID:24374776

Measurement of the performance of a spiral wound polyimide regenerator in a pulse tube refrigerator

NASA Technical Reports Server (NTRS)

Rawlins, Wayne; Timmerhaus, Klaus D.; Radebaugh, Ray; Daney, D. E.

1991-01-01

A regenerator for use in a pulse tube refrigerator has been constructed from a polyimide (polypyromellitimide or PPMI) whose small ratio of thermal conductivity to heat capacity make it a good candidate for a regenerator material in cryocoolers. The regenerator was fabricated using 25 micron thick photoresist strips bonded to a 50 micron thick sheet of PPMI. This composite sheet was wound in jelly-roll fashion around a mandrel and inserted into the regenerator housing. The photoresist strips, formed using a photolithographic technique, provided a 25 micron spacing for the axial flow of gas between each layer of PPMI. Ineffectiveness results are presented for this material under actual operating conditions in a pulse tube refrigerator and compared with a numerical model. The numerical model indicated that a polyimide regenerator would perform much better than one constructed of stainless steel screen, but the experimental results showed the opposite behavior. Measured values for the ineffectiveness were 0.003 for the stainless steel screen and 0.017 for the polyimide.

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.

Molecular beam scattering from C-13 enriched Kapton and correlation with the EOIM-3 carousel experiment

NASA Technical Reports Server (NTRS)

Minton, Timothy K.; Moore, Teresa A.

1995-01-01

Mass spectra of products emerging from identical samples of a C-13-enriched polyimide polymer (chemically equivalent to Kapton) under atomic oxygen bombardment in space and in the laboratory were collected. Reaction products unambiguously detected in space were CO-13, NO, (12)CO2, and (13)CO2. These reaction products and two others, H2O and CO-12, were detected in the laboratory, along with inelastically scattered atomic and molecular oxygen. Qualitative agreement was seen in the mass spectra taken in space and in the laboratory; the agreement may be improved by reducing the fraction of O2 in the laboratory molecular beam. Both laboratory and space data indicated that CO and CO2 products come preferentially from reaction with the imide component of the polymer chain, raising the possibility that the either component may degrade in part by the 'evaporation' of higher molecular weight fragments. Laboratory time-of-flight distributions showed: (1) incomplete energy accommodation of impinging O and O2 species that do not react with the surface; and (2) both hyperthermal and thermal CO and CO2 products, suggesting two distinct reaction mechanisms with the surface.

Phosphorus-containing imide resins

NASA Technical Reports Server (NTRS)

Varma, I. K.; Fohlen, G. M.; Parker, J. A. (Inventor)

1984-01-01

Flame-resistant reinforced bodies are disclosed which are composed of reinforcing fibers, filaments or fabrics in a cured body of bis- and tris-imide resins derived from tris(m-aminophenyl) phosphine oxides by reaction with maleic anhydride or its derivatives, or of addition polymers of such imides, including a variant in which a mono-imide is condensed with a dianhydride and the product is treated with a further quantity of maleic anhydride.

Polarization Stability of Amorphous Piezoelectric Polyimides

NASA Technical Reports Server (NTRS)

Park, C.; Ounaies, Z.; Su, J.; Smith, J. G., Jr.; Harrison, J. S.

2000-01-01

Amorphous polyimides containing polar functional groups have been synthesized and investigated for potential use as high temperature piezoelectric sensors. The thermal stability of the piezoelectric effect of one polyimide was evaluated as a function of various curing and poling conditions under dynamic and static thermal stimuli. First, the polymer samples were thermally cycled under strain by systematically increasing the maximum temperature from 50 C to 200 C while the piezoelectric strain coefficient was being measured. Second, the samples were isothermally aged at an elevated temperature in air, and the isothermal decay of the remanent polarization was measured at room temperature as a function of time. Both conventional and corona poling methods were evaluated. This material exhibited good thermal stability of the piezoelectric properties up to 100 C.

Tribological Evaluation of Candidate Gear Materials Operating Under Light Loads in Highly Humid Conditions

NASA Technical Reports Server (NTRS)

Dellacorte, Christopher; Thomas, Fransua; Leak, Olivia Ann

2015-01-01

A series of pin-on-disk sliding wear tests were undertaken to identify candidate materials for a pair of lightly loaded timing gears operating under highly humid conditions. The target application involves water purification and thus precludes the use of oil, grease and potentially toxic solid lubricants. The baseline sliding pair is austenitic stainless steel operating against a carbon filled polyimide. The test load and sliding speed (4.9 N, 2.7 m/s) were chosen to represent average contact conditions of the meshing gear teeth. In addition to the baseline materials, the hard superelastic NiTiNOL 60 (60NiTi) was slid against itself, against the baseline polyimide, and against 60NiTi onto which a commercially deposited dry film lubricant (DFL) was applied. The alternate materials were evaluated as potential replacements to achieve a longer wear life and improved dimensional stability for the timing gear application. An attempt was also made to provide solid lubrication to self-mated 60NiTi by rubbing the polyimide against the disk wear track outside the primary 60NiTi-60NiTi contact, a method named stick or transfer-film lubrication. The selected test conditions gave repeatable friction and wear data and smooth sliding surfaces for the baseline materials similar to those in the target application. Friction and wear for self-mated stainless steel were high and erratic. Self-mated 60NiTi gave acceptably low friction (approx. 0.2) and modest wear but the sliding surfaces were rough and potentially unsuitable for the gear application. Tests in which 60NiTi pins were slid against DFL coated 60NiTi and DFL coated stainless steel gave low friction and long wear life. The use of stick lubrication via the secondary polyimide pin provided effective transfer film lubrication to self-mated 60NiTi tribological specimens. Using this approach, friction levels were equal or lower than the baseline polyimide-stainless combination and wear was higher but within data scatter observed in these preliminary tests. Based upon these results, self-mated 60NiTi gear teeth utilizing solid lubrication, is a reasonable approach for the target application.

Tribological Evaluation of Candidate Gear Materials Operating Under Light Loads in Highly Humid Conditions

NASA Technical Reports Server (NTRS)

DellaCorte, Christopher; Thomas, Fransua; Leak, Olivia Ann

2015-01-01

A series of pin-on-disk sliding wear tests were undertaken to identify candidate materials for a pair of lightly loaded timing gears operating under highly humid conditions. The target application involves water purification and thus precludes the use of oil, grease and potentially toxic solid lubricants. The baseline sliding pair is austenitic stainless steel operating against a carbon filled polyimide. The test load and sliding speed (4.9N, 2.7ms) were chosen to represent average contact conditions of the meshing gear teeth. In addition to the baseline materials, the hard superelastic NiTiNOL 60 (60NiTi) was slid against itself, against the baseline polyimide, and against 60NiTi onto which a commercially deposited dry film lubricant (DFL) was applied. The alternate materials were evaluated as potential replacements to achieve a longer wear life and improved dimensional stability for the timing gear application. An attempt was also made to provide solid lubrication to self-mated 60NiTi by rubbing the polyimide against the disk wear track outside the primary 60NiTi-60NiTi contact, a method named stick or transfer-film lubrication. The selected test conditions gave repeatable friction and wear data and smooth sliding surfaces for the baseline materials similar to those in the target application. Friction and wear for self-mated stainless steel were high and erratic. Self-mated 60NiTi gave acceptably low friction (0.2) and modest wear but the sliding surfaces were rough and potentially unsuitable for the gear application. Tests in which 60NiTi pins were slid against DFL coated 60NiTi and DFL coated stainless steel gave low friction and long wear life. The use of stick lubrication via a secondary polyimide pin provided effective transfer film lubrication to self-mated 60NiTi tribological specimens. Using this approach, friction levels were equal or lower than the baseline polyimide-stainless combination and wear was higher but within data scatter observed in these preliminary tests. Based upon these results, self-mated 60NiTi gear teeth utilizing solid lubrication, is a reasonable approach for the target application.

Preparation of Imide Oligomers via Concurrent Reactive Extrusion

NASA Technical Reports Server (NTRS)

Avakian, Roger W. (Inventor); Hu, Ling (Inventor)

2018-01-01

Reactive extrusion can be used in a continuous, solvent-less preparation of imide oligomers involving two competing reactions among three ingredients, the first reaction between a dianhydride and a diamine and the second reaction between an endcap and the same diamine. The imide oligomer can form a composite via conventional production methods or via formation of a film from imide oligomer re-melted in an extruder before being impregnated into tape or fabric.

Process for preparing phthalocyanine polymer from imide containing bisphthalonitrile

NASA Technical Reports Server (NTRS)

Achar, Bappalige N. (Inventor); Fohlen, George M. (Inventor); Parker, John A. (Inventor)

1987-01-01

Imide-linked bisphthalonitrile compounds are prepared by combining a dicyano aromatic diamine and an organic dianhydride to produce an amic acid linked bisphthalonitrile compound. The amic acid linked bisphthalonitrile compound is dehydrocyclized to produce the imide-linked bisphthalonitrile compounds. The imide-linked bisphthalonitrile compounds may be polymerized to produce a phythalocyanine polymer by heating the imide-linked bisphthalonitrile compound, either alone or in the presence of a metal powder or a metal salt. These compounds are useful in the coating, laminating and molding arts. The polymers are useful in composite matrix resins where increased fire resistance, toughness and resistance to moisture are required, particularly as secondary structures in aircraft and spacecraft.

Imide/arylene ether block copolymers

NASA Technical Reports Server (NTRS)

Jensen, B. J.; Hergenrother, P. M.; Bass, R. G.

1991-01-01

Two series of imide/arylene either block copolymers were prepared using an arylene ether block and either an amorphous or semi-crystalline imide block. The resulting copolymers were characterized and selected physical and mechanical properties were determined. These results, as well as comparisons to the homopolymer properties, are discussed.

Implementing Integrated Multicultural Instructional Design in Management Education

ERIC Educational Resources Information Center

Schultz, Jennifer L.; Higbee, Jeanne L.

2011-01-01

This purpose of this paper is to summarize the principles of integrated multicultural instructional design (IMID; Higbee, Goff, & Schultz, in press; Higbee, Schultz, & Goff, 2010) and present specific strategies for incorporating IMID in management education. The primary goal of IMID is to promote the integration of multicultural content…

Imide/arylene ether copolymers with pendent trifluoromethyl groups

NASA Technical Reports Server (NTRS)

Jensen, Brian J.; Havens, Stephen J.

1992-01-01

A series of imide/arylene ether block copolymers were prepared using an arylene ether block containing a hexafluoroisopropylidene group and an imide block containing a hexafluoroisopropylidene and a trifluoromethyl group in the polymer backbone. The copolymers were characterized and mechanical properties were determined and compared to the homopolymers.

The Gut Microbiota in Immune-Mediated Inflammatory Diseases

PubMed Central

Forbes, Jessica D.; Van Domselaar, Gary; Bernstein, Charles N.

2016-01-01

The collection of microbes and their genes that exist within and on the human body, collectively known as the microbiome has emerged as a principal factor in human health and disease. Humans and microbes have established a symbiotic association over time, and perturbations in this association have been linked to several immune-mediated inflammatory diseases (IMID) including inflammatory bowel disease, rheumatoid arthritis, and multiple sclerosis. IMID is a term used to describe a group of chronic, highly disabling diseases that affect different organ systems. Though a cornerstone commonality between IMID is the idiopathic nature of disease, a considerable portion of their pathobiology overlaps including epidemiological co-occurrence, genetic susceptibility loci and environmental risk factors. At present, it is clear that persons with an IMID are at an increased risk for developing comorbidities, including additional IMID. Advancements in sequencing technologies and a parallel explosion of 16S rDNA and metagenomics community profiling studies have allowed for the characterization of microbiomes throughout the human body including the gut, in a myriad of human diseases and in health. The main challenge now is to determine if alterations of gut flora are common between IMID or, if particular changes in the gut community are in fact specific to a single disease. Herein, we review and discuss the relationships between the gut microbiota and IMID. PMID:27462309

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.

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.

Crystalline imide/arylene ether copolymers

NASA Technical Reports Server (NTRS)

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

1995-01-01

Crystalline imide/arylene ether block copolymers are prepared by reacting anhydride terminated poly(amic acids) with amine terminated poly)arylene ethers) in polar aprotic solvents and chemically or thermally cyclodehydrating the resulting intermediate poly(amic acids). The block copolymers of the invention have one glass transition temperature or two, depending on the particular structure and/or the compatibility of the block units. Most of these crystalline block copolymers for tough, solvent resistant films with high tensile properties. While all of the copolymers produced by the present invention are crystalline, testing reveals that copolymers with longer imide blocks or higher imide content have increased crystallinity.

Phosphorus-containing imide resins

NASA Technical Reports Server (NTRS)

Varma, I. K.; Fohlen, G. M.; Parker, J. A. (Inventor)

1983-01-01

Bis- and tris-imides derived from tris (m-aminophenyl) phosphine oxides by reaction with maleic anhydride or its derivatives, and addition polymers of such imides, including a variant in which a mono-imide is condensed with a dianhydride and the product is treated with a further quantity of maleic anhydride. Such monomers or their oligomes may be used to impregnate fibers and fabrics which when cured, are flame resistant. Also an improved method of producing tris (m-aminophenyl) phosphine oxides from the nitro analogues by reduction with hydrazine hydrate using palladized charcoal or Raney nickel as the catalyst is described.

Effectiveness of educational outreach in infectious diseases management: a cluster randomized trial in Uganda.

PubMed

Mbonye, Martin Kayitale; Burnett, Sarah M; Naikoba, Sarah; Ronald, Allan; Colebunders, Robert; Van Geertruyden, Jean-Pierre; Weaver, Marcia R

2016-08-04

Integrated Infectious Diseases Capacity Building Evaluation (IDCAP) teams designed and implemented two health worker in-service training approaches: 1) an off-site classroom-based integrated management of infectious diseases (IMID) course with distance learning aspects, and 2) on-site support (OSS), an educational outreach intervention. We tested the effects of OSS on workload and 12 facility performance indicators for emergency triage assessment and treatment, HIV testing, and malaria and pneumonia case management among outpatients by two subgroups: 1) mid-level practitioners (MLP) who attended IMID training (IMID-MLP) and 2) health workers who did not (No-IMID). Thirty-six health facilities participated in the IDCAP trial, with 18 randomly assigned to Arm A and 18 to Arm B. Two MLP in both arms received IMID. All providers at Arm A facilities received nine monthly OSS visits from April to December 2010 while Arm B did not. From November 2009 to December 2010, 777,667 outpatient visits occurred. We analyzed 669,580 (86.1 %) outpatient visits, where provider cadre was reported. Treatment was provided by 64 IMID-MLP and 1,515 No-IMID providers. The effect of OSS was measured by the difference in pre/post changes across arms after controlling for covariates (adjusted ratio of relative risks = a RRR). The effect of OSS on patients-per-provider-per-day (workload) among IMID-MLP (aRRR = 1.21; p = 0.48) and No-IMID (aRRR = 0.90; p = 0.44) was not statistically significant. Among IMID-MLP, OSS was effective for three indicators: malaria cases receiving an appropriate antimalarial (aRRR = 1.26, 99 % CI = 1.02-1.56), patients with negative malaria test result prescribed an antimalarial (aRRR = 0.49, 99 % CI = 0.26-0.92), and patients with acid-fast bacilli smear negative result receiving empiric treatment for acute respiratory infection (aRRR = 2.04, 99 % CI = 1.06-3.94). Among No-IMID, OSS was effective for two indicators: emergency and priority patients admitted, detained or referred (aRRR = 2.12, 99 % CI = 1.05-4.28) and emergency patients receiving at least one appropriate treatment (aRRR = 1.98, 99 % CI = 1.21-3.24). Effects of OSS on workload were not statistically significant. Significant OSS effects on facility performance across subgroups were heterogeneous. OSS supported MLP who diagnosed and treated patients to apply IMID knowledge. For other providers, OSS supported team work to manage emergency patients. This evidence on OSS effectiveness could inform interventions to improve health workers' capacity to deliver better quality infectious diseases care.

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.

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.

Studies on the intramolecular cyclizations of bicyclic delta-hydroxynitriles promoted by triflic anhydride.

PubMed

Justribó, Valeria; Pellegrinet, Silvina C; Colombo, María I

2007-05-11

Studies have been conducted to investigate the reactivity of several bicyclic delta-hydroxynitriles with triflic anhydride in dichloromethane. The reactions of the analogues derived from 1-indanone and 1-tetralone lead to annulated enones. These products arise from an initial elimination reaction that generates an alkene, followed by the addition of the carbon-carbon double bond to the activated cyano group. The intramolecular cyclization of the derivative obtained from 1-benzosuberone unexpectedly followed a different path, giving a cyclic imidate as the major product. In this case, the activated cyano group is directly attacked by the hydroxyl group of the starting delta-hydroxynitrile. Theoretical calculations provide a rationale for the observed reactivity pattern. Both the formation of the triflate via its protonated form, its subsequent ionization to the carbocation, and the cyclization of the resulting alkene to the enone become less favorable when the size of the ring increases due to conformational effects. The opposite trend is observed for the competing Pinner-type cyclization to the imidate. An alternative mechanism for the formation of the lactams from the cyclic imidates under acid-catalyzed conditions has also been proposed.

Organo-modified anionic clays into polymer compared to smectite-type nanofiller: potential applications of the nanocomposites.

PubMed

Leroux, Fabrice

2006-02-01

The scope of the article is to provide the state of the art concerning the utilization of Layered Double Hydroxide (LDH) materials in polymer nanocomposite and to enlight their potential application and even advantage in comparison to smectite-type materials. A particular attention is paid on the synthetic procedures for the elaboration of polymer nanocomposite taking poly(styrene), poly(imide), poly(methylmethacrylate) and epoxy resin as examples. Lipophilization of the inorganic platelets used to decrease the surface polarity may be achieved either with a surfactant molecule or a surfactant monomer molecule, giving rise to reactive hybrid filler. The state of dispersion of the inorganic platelets, i.e., intercalated versus exfoliated structure is discussed. LDH-based nanocomposites present mechanical properties, such as the tensile modulus and elongation at break, always greater in comparison to virgin polymer, but also compete well with smectite-type filler. For epoxy nanocomposite, the relative gain using LDH nanofiller is superior to smectite-type filler. In both types of nanocomposites using either LDH or smectite-type nanofiller, mixed intercalated-exfoliated structure is generally met. Dispersion of LDH nanoplatelets should emerge well as flame-retardant materials and as polymer electrolyte, but may also find application in topical domains such as in sun radiation absorption.

A critical study of the role of the surface oxide layer in titanium bonding

NASA Technical Reports Server (NTRS)

Dias, S.; Wightman, J. P.

1983-01-01

Scanning electron microscope/X-ray photoelectron spectroscopy (SEM/XPS) analysis of fractured adhesively bonded Ti 6-4 samples is discussed. The text adhesives incuded NR 056X polyimide, polypheylquinoxaline (PPQ), and LARC-13 polyimide. Differentiation between cohesive and interfacial failure was based on the absence of presence of a Ti 2p XPS photopeak. In addition, the surface oxide layer on Ti-(6A1-4V) adherends is characterized and bond strength and durability are addressed. Bond durability in various environmental conditions is discussed.

Low dielectric polyimide fibers

NASA Technical Reports Server (NTRS)

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

1994-01-01

A high temperature resistant polyimide fiber that has a dielectric constant of less than 3 is presented. The fiber was prepared by first reacting 2,2-bis (4-(4aminophenoxy)phenyl) hexafluoropropane with 2,2-bis (3,4-dicarboxyphenyl) hexafluoropropane dianhydride in an aprotic solvent to form a polyamic acid resin solution. The polyamic acid resin solution is then extruded into a coagulation medium to form polyamic acid fibers. The fibers are thermally cured to their polyimide form. Alternatively, 2,2-bis(4-(4-aminophenoxy)phenyl) hexafluoropropane is reacted with 2,2-bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride to form a polyamic acid, and the polyamic acid is chemically converted to its polyimide form. The polyimide is then dissolved in a solvent to form a polyimide resin solution, and the polyimide resin is extruded into a coagulation medium to form a polyimide wet gel filament. In order to obtain polyimide fibers of increased tensile properties, the polyimide wet gel filaments are stretched at elevated temperatures. The tensile properties of the fibers were measured and found to be in the range of standard textile fibers. Polyimide fibers obtained by either method will have a dielectric constant similar to that of the corresponding polymer, viz., less than 3 at 10 GHz.

Optical fiber sensors based on novel polyimide for humidity monitoring of building materials

NASA Astrophysics Data System (ADS)

Chai, Jing; Liu, Qi; Liu, Jinxuan; Zhang, Dingding

2018-03-01

This paper presents novel preparation methods of polyimide and coupling agent, coated on the fiber Bragg grating (FBG) sensor for monitoring relative humidity (RH). The sensing mechanism that the volume change of the moisture-sensitive polyimide induces the shift of the Bragg wavelength of FBG is used in the RH sensor. The performance of the polymer-coated RH sensor was evaluated under laboratory conditions of temperature over a range of values (20.0-80.0 °C) and humidity over a range of RH values (25.0-95.0%). The time response and RH sensitivity of the sensor based on novel polyimide and coupling agent was improved, compared to the previous. A new packaged RH sensor was designed, which was used in detecting the moisture diffusion and evolutions inside of sample made of building materials which exposed to a controlled environment in the lab after casting. Relative humidity inside of sample with time was 100% in the first phase of vapor-saturated, slowly reduced in the latter phase. The results indicate the RH sensor developed provides a feasible method to detect the influence of environment on moisture inside the material in the drying process.

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).

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.

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.

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.

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.

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.

Comparative study of imide-based Li salts as electrolyte additives for Li-ion batteries

NASA Astrophysics Data System (ADS)

Sharova, Varvara; Moretti, Arianna; Diemant, Thomas; Varzi, Alberto; Behm, R. Jürgen; Passerini, Stefano

2018-01-01

Herein, we report the results of a detailed study on the use of different Li imide salts (LiTFSI, LiFSI, and LiFTFSI) as electrolyte additives for lithium-ion batteries. The introduction of lithium imide salts in the electrolyte is shown to considerably improve the first cycle coulombic efficiency and the long-term cycling stability of graphite/LiFePO4 cells. Using LiTFSI, a capacity fading of only ∼2% occurred over 600 cycles while the control cell with the state-of-the-art additive (VC) lost ∼20% of the initial capacity at 20 °C. The results of the XPS and impedance spectroscopy measurements of graphite electrodes show that, after the formation cycle, the SEI obtained in the presence of imide salts is thinner, contains more LiF and is less resistive than that obtained using VC. Despite the beneficial effect of the imide salts on the lithium-ion cell performance, a slightly reduced thermal stability of the SEI is observed.

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.

Kaolinite Nanocomposite Platelets Synthesized by Intercalation and Imidization of Poly(styrene-co-maleic anhydride)

PubMed Central

Samyn, Pieter; Schoukens, Gustaaf; Stanssens, Dirk

2015-01-01

A synthesis route is presented for the subsequent intercalation, exfoliation and surface modification of kaolinite (Kln) by an imidization reaction of high-molecular weight poly(styrene-co-maleic anhydride) or SMA in the presence of ammonium hydroxide. In a first step, the intercalation of ammonolyzed SMA by guest displacement of intercalated dimethylsulfoxide has been proven. In a second step, the imidization of ammonolyzed SMA at 160 °C results in exfoliation of the kaolinite layers and deposition of poly(styrene-co-maleimide) or SMI nanoparticles onto the kaolinite surfaces. Compared with a physical mixture of Kln/SMI, the chemically reacted Kln/SMI provides more efficient exfoliation and hydrogen bonding between the nanoparticles and the kaolinite. The kaolinite nanocomposite particles are synthesized in aqueous dispersion with solid content of 65 wt %. The intercalation and exfoliation are optimized for a concentration ratio of Kln/SMI = 70:30, resulting in maximum intercalation and interlayer distance in combination with highest imide content. After thermal curing at 135 °C, the imidization proceeds towards a maximum conversion of the intermediate amic acid moieties. The changes in O–H stretching and kaolinite lattice vibrations have been illustrated by infrared and FT-Raman spectroscopy, which allow for a good quantification of concentration and imidization effects. PMID:28793445

Molecular mechanism of action of immune-modulatory drugs thalidomide, lenalidomide and pomalidomide in multiple myeloma

PubMed Central

Zhu, Yuan Xiao; Kortuem, K. Martin; Stewart, A. Keith

2014-01-01

Although several mechanisms have been proposed to explain the activity of thalidomide, lenalidomide and pomalidomide in multiple myeloma (MM), including demonstrable anti-angiogenic, anti-proliferative and immunomodulatory effects, the precise cellular targets and molecular mechanisms have only recently become clear. A landmark study recently identified cereblon (CRBN) as a primary target of thalidomide teratogenicity. Subsequently it was demonstrated that CRBN is also required for the anti-myeloma activity of thalidomide and related drugs, the so-called immune-modulatory drugs (IMiDs). Low CRBN expression was found to correlate with drug resistance in MM cell lines and primary MM cells. One of the downstream targets of CRBN identified is interferon regulatory factor 4 (IRF4), which is critical for myeloma cell survival and is down-regulated by IMiD treatment. CRBN is also implicated in several effects of IMiDs, such as down-regulation of tumor necrosis factor-α (TNF-α) and T cell immunomodulatory activity, demonstrating that the pleotropic actions of the IMiDs are initiated by binding to CRBN. Future dissection of CRBN downstream signaling will help to delineate the underlying mechanisms for IMiD action and eventually lead to development of new drugs with more specific anti-myeloma activities. It may also provide a biomarker to predict IMiD response and resistance. PMID:22966948

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.

Adherence to systemic therapies for immune-mediated inflammatory diseases in Lebanon: a physicians' survey from three medical specialties.

PubMed

Ammoury, Alfred; Okais, Jad; Hobeika, Mireille; Sayegh, Raymond B; Shayto, Rani H; Sharara, Ala I

2017-01-01

Immune-mediated inflammatory diseases (IMIDs) are chronic conditions that may cause tissue damage and disability, reduced quality of life and increased mortality. Various treatments have been developed for IMIDs, including immune modulators and targeted biologic agents. However, adherence remains suboptimal. An adherence survey was used to evaluate physicians' beliefs about adherence to medication in IMID and to evaluate if and how they manage adherence. The survey was distributed to 100 randomly selected physicians from three different specialties. Results were analyzed by four academic experts commissioned to develop an action plan to address practical and perceptual barriers to adherence, integrating it into treatment goals to maximize outcomes in IMID, thereby elevating local standards of care. Eighty-two physicians participated in this study and completed the questionnaire. Most defined adherence as compliance with prescribed treatment. Although the majority of surveyed physicians (74%) did not systematically measure adherence in their practice, 54% identified adherence as a treatment goal of equal or greater importance to therapeutic endpoints. Lack of time and specialized nursing support was reported as an important barrier to measuring adherence. The expert panel identified four key areas for action: 360° education (patient-nurse-physician), patient-physician communication, patient perception and concerns, and market access/cost. An action plan was developed centered on education and awareness, enhanced benefit-risk communication, development of adherence assessment tools and promotion of patient support programs. Nonadherence to medication is a commonly underestimated problem with important consequences. A customized target-based strategy to address the root causes of non-adherence is essential in the management of chronic immune-mediated diseases.

Development of autoclavable addition type polyimides

NASA Technical Reports Server (NTRS)

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

1974-01-01

Two highly promising approaches to yield autoclavable addition-type polyimides were identified and evaluated in the program. Conditions were established for autoclave preparation of Hercules HMS graphite fiber reinforced composites in the temperature range of 473 K to 505 K under an applied pressure of 0.7 MN/m2 (100 psi) for time durations up to four hours. Upon oven postcure in air at 589 K, composite samples demonstrated high mechanical property retention at 561 K after isothermal aging in air for 1000 hours. Promise was shown for shorter term mechanical property retention at 589 K upon exposure in air at this temperature.

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: Thermally stable aerospace polymers

NASA Technical Reports Server (NTRS)

St.clair, A. K.

1980-01-01

An up to date review of available commercial and experimental high temperature polyimide resins which show potential for aerospace applications is presented. Current government research trends involving the use of polyimides as matrix resins for structural composites are discussed. Both the development of polyimides as adhesives for bonding metals and composites, and as films and coatings for use in an aerospace environment are reviewed. In addition, future trends for polyimides are proposed.

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.

A possible role of polycystic ovary syndrome for pregnancy complications in women with psoriasis.

PubMed

De Simone, Clara; Caldarola, Giacomo; Corbeddu, Marialuisa; Moro, Francesca; Tropea, Anna; Moretta, Gaia; Apa, Rosanna

2014-11-01

Psoriasis is a common, chronic, relapsing immune-mediated inflammatory disease (IMID) of the skin. IMIDs are multifactorial diseases characterized by common molecular pathways leading to a systemic inflammation. Patients with an IMID are also at higher risk of developing co-morbidities, such as adverse pregnancy outcomes, than the general population. A higher rate of pregnancy complications have been seen in inflammatory bowel disease and rheumatoid arthritis. The data for psoriasis are inconsistent but it appears that women with moderate-to-severe psoriasis may also have an increased risk of poor pregnancy outcomes. The cause of this association is unknown, although it may be related to elevated proinflammatory cytokines such as IL-6 and TNF-α, the high prevalence of comorbidities and other unhealthy behaviours, or the high prevalence of polycystic ovary syndrome (PCOS). In a recent study, PCOS prevalence in a psoriatic cohort (n = 51) was higher than in non-psoriatic women (n = 102) (47% versus 11%), and women with PCOS and psoriasis had a greater probability of insulin resistance, hyperinsulinaemia, and dyslipidaemia as well as a more severe skin condition, than those with psoriasis alone. Further studies are necessary to clarify the impact of psoriasis on pregnancy and in particular if these effects are mediated by concomitant PCOS. © 2014 Wiley Periodicals, Inc.

Impact of silver metallization and electron irradiation on the mechanical deformation of polyimide films

NASA Astrophysics Data System (ADS)

Muradov, A. D.; Mukashev, K. M.; Yar-Mukhamedova, G. Sh.; Korobova, N. E.

2017-11-01

The impact of silver metallization and electron irradiation on the physical and mechanical properties of polyimide films has been studied. The metal that impregnated the structure of the polyimide substrate was 1-5 μm. The surface coatings contained 80-97% of the relative silver mirror in the visible and infrared regions. Irradiation was performed at the ELU-6 linear accelerator with an average beam electron energy of 2 MeV, an integral current of up to 1000 μA, a pulse repetition rate of 200 Hz, and a pulse duration of 5 μs. The absorbed dose in the samples was 10, 20, 30, and 40 MGy. The samples were deformed at room temperature under uniaxial tension on an Instron 5982 universal testing system. The structural changes in the composite materials that result from the impact of the physical factors were studied using an X-ray diffractometer DRON-2M in air at 293 K using Cu K α radiation (λαCu = 1.5418 Å). A substantial growth of mechanical characteristics resulting from the film metallization, as compared to the pure film, was observed. The growth of the ultimate strength by Δσ = 105 MPa and the plasticity by Δɛ = 75% is connected with the characteristics of the change of structure of the metallized films and the chemical etching conditions. The electron irradiation of the metallized polyimide film worsens its elastic and strength characteristics due to the formation of new phases in the form of silver oxide in the coating. The concentration of these phases increased with increasing dose, which was also the result of the violation of the ordered material structure, namely, the rupture of polyimide macromolecule bonds and the formation of new phases of silver in the coating. A mathematical model was obtained that predicts the elastic properties of silver metallized polyimide films. This model agrees with the experimental data.

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.

Structure-Property Relationship in High Tg Thermosetting Polyimides

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.; Meador, Mary Ann B.; HardyGreen, DeNise

2000-01-01

This viewgraph presentation gives an overview of the structure-property relationship in high glass transition temperatures (T(sub g)) thermosetting polyimides. The objectives of this work are to replace MDA in PMR-15 with 2,2-substituted benzidine and to evaluate the thermo-oxidative stability and mechanical properties of DMBZ-15 against PMR-15. Details are given on the T(sub g) of polyimide resins, the x-ray crystal structure of 2,2-Bis(trifluoro)benzidine (BFBZ), the isothermal aging of polyimide resins at 288 C under 1 atm of circulating air, the compressive strength of polyimide composites, and a gas evaluation profile of DMBZ-15 polyimide resins.

Immunomodulatory drugs disrupt the cereblon-CD147-MCT1 axis to exert antitumor activity and teratogenicity.

PubMed

Eichner, Ruth; Heider, Michael; Fernández-Sáiz, Vanesa; van Bebber, Frauke; Garz, Anne-Kathrin; Lemeer, Simone; Rudelius, Martina; Targosz, Bianca-Sabrina; Jacobs, Laura; Knorn, Anna-Maria; Slawska, Jolanta; Platzbecker, Uwe; Germing, Ulrich; Langer, Christian; Knop, Stefan; Einsele, Herrmann; Peschel, Christian; Haass, Christian; Keller, Ulrich; Schmid, Bettina; Götze, Katharina S; Kuster, Bernhard; Bassermann, Florian

2016-07-01

Immunomodulatory drugs (IMiDs), such as thalidomide and its derivatives lenalidomide and pomalidomide, are key treatment modalities for hematologic malignancies, particularly multiple myeloma (MM) and del(5q) myelodysplastic syndrome (MDS). Cereblon (CRBN), a substrate receptor of the CRL4 ubiquitin ligase complex, is the primary target by which IMiDs mediate anticancer and teratogenic effects. Here we identify a ubiquitin-independent physiological chaperone-like function of CRBN that promotes maturation of the basigin (BSG; also known as CD147) and solute carrier family 16 member 1 (SLC16A1; also known as MCT1) proteins. This process allows for the formation and activation of the CD147-MCT1 transmembrane complex, which promotes various biological functions, including angiogenesis, proliferation, invasion and lactate export. We found that IMiDs outcompete CRBN for binding to CD147 and MCT1, leading to destabilization of the CD147-MCT1 complex. Accordingly, IMiD-sensitive MM cells lose CD147 and MCT1 expression after being exposed to IMiDs, whereas IMiD-resistant cells retain their expression. Furthermore, del(5q) MDS cells have elevated CD147 expression, which is attenuated after IMiD treatment. Finally, we show that BSG (CD147) knockdown phenocopies the teratogenic effects of thalidomide exposure in zebrafish. These findings provide a common mechanistic framework to explain both the teratogenic and pleiotropic antitumor effects of IMiDs.

Immunomodulatory drugs and the risk of serious infection in multiple myeloma: systematic review and meta-analysis of randomized and observational studies.

PubMed

Chen, Min; Zhao, Yongfeng; Xu, Chuanxin; Wang, Xian; Zhang, Xianping; Mao, Benyu

2018-06-01

The effect of immunomodulatory drugs (IMiDs) on serious infection remains uncertain. We therefore conducted a systematic review and meta-analysis to assess the possible impact of IMiDs on serious infection in patients with multiple myeloma (MM). We searched randomized controlled trials (RCTs) and observational studies from databases that addressed the effect of IMiDs on serious infection in patients with MM. We pooled data from RCTs and observational studies separately and used the GRADE approach to rate the quality of evidence. Rates in patients with individual IMiDs at different treatment status ranged from 7.00 to 23.00%. The use of thalidomide- or lenalidomide-based regimen induction therapy for autologous stem cell transplantation (ASCT)-ineligible patients suggests increase in serious infection (RR = 1.59, 95% CI 1.31-1.93, p < 0.01). Compared to conventional therapy, IMiDs' induction in ASCT-eligible patients significantly decreases the risk of serious infection (RR = 0.82, 95% CI 0.72-0.94, p < 0.01). Lenalidomide-based therapy was associated with a significant increase in risk of serious infection in patients treated compared with conventional therapy (RR = 2.45, 95% CI 1.57-3.83, p < 0.01). The current evidence suggests that patients with MM treated with IMiDs are at a high risk of serious infection.

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

Chemistry and Properties of Imide Oligomers from Phenylethynyl-Containing Diamines

NASA Technical Reports Server (NTRS)

Smith, J. G., Jr.; Connell, J. W.

2000-01-01

As an extension of work on pendent phenylethynlyl-containing imide oligomer, three new diamines containing pendent phenylethynyl groups were prepared and characterized. These diamines were used to prepare pendent and pendent and terminal phenylethynyl imide oliogomers via the amide acid route in N-methyl-2-pyrrolidinone at a calculated number average molecular weight of 5000 g mol (exp -1). The pendent phenylethynyl groups were randomly distributed along the oliogomer backbone and provided a means of controlling the distance between reactive sites. The imide oligomers were characterized and thermally cured, and the cured polymers evaluated as thin films and compared with materials of similar composition prepared from 3,5-diamino-4'-phenylethynylbenzophenone. This work was performed as part of a continuing research effort to develop structural resins for potential aeronautical applications.

Decomposition of poly(amide-imide) film enameled on solid copper wire using atmospheric pressure non-equilibrium plasma.

PubMed

Sugiyama, Kazuo; Suzuki, Katsunori; Kuwasima, Shusuke; Aoki, Yosuke; Yajima, Tatsuhiko

2009-01-01

The decomposition of a poly(amide-imide) thin film coated on a solid copper wire was attempted using atmospheric pressure non-equilibrium plasma. The plasma was produced by applying microwave power to an electrically conductive material in a gas mixture of argon, oxygen, and hydrogen. The poly(amide-imide) thin film was easily decomposed by argon-oxygen mixed gas plasma and an oxidized copper surface was obtained. The reduction of the oxidized surface with argon-hydrogen mixed gas plasma rapidly yielded a metallic copper surface. A continuous plasma heat-treatment process using a combination of both the argon-oxygen plasma and argon-hydrogen plasma was found to be suitable for the decomposition of the poly(amide-imide) thin film coated on the solid copper wire.

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.

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.

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.

Rheological characterization of addition polyimide matrix resins and prepregs

NASA Technical Reports Server (NTRS)

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

1984-01-01

Although graphite-reinforced polyimide matrix composites offer outstanding specific strength and stiffness, together with high thermal oxidative stability, processing problems connected with their rheological behavior remain to be addressed. The present rheological studies on neat polyimide resin systems encountered outgassing during cure. A staging technique has been developed which can successfully handle polyimide samples, and novel methods were applied to generate rheological curves for graphite-reinforced prepregs. The commercial graphite/polyimide systems studied were PRM 15, LARC 160, and V378A.

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

21 CFR 177.2450 - Polyamide-imide resins.

Code of Federal Regulations, 2011 CFR

2011-04-01

... than 500 parts per million. Residual monomers are determined by gas chromatography (the gas chromatography method titled “Amide-Imide Polymer Analysis—Analysis of Monomer Content,” is incorporated by...

21 CFR 177.2450 - Polyamide-imide resins.

Code of Federal Regulations, 2014 CFR

2014-04-01

... polyamide-imide resins are derived from the condensation reaction of substantially equimolar parts of.... 31957-38-7) derived from the condensation reaction of equimolar parts of benzoyl chloride-3,4...

Cooperative dual catalysis: application to the highly enantioselective conjugate cyanation of unsaturated imides.

PubMed

Sammis, Glenn M; Danjo, Hiroshi; Jacobsen, Eric N

2004-08-18

Cooperative heterobimetallic catalysis was used as a design principle to achieve a highly reactive system for the enantioselective conjugate addition of cyanide to alpha,beta-unsaturated imides. A dual-catalyst pathway involving chiral (salen)Al complex 1b and chiral (pybox)Er complex 4b provides measurable improvements in rates and enantioselectivities relative to single-catalyst systems. Mechanistic studies point to a cooperative bimetallic mechanism involving activation of the imide by the Al complex and activation of cyanide by the Er complex.

Electrically conductive resinous bond and method of manufacture

DOEpatents

Snowden, T.M. Jr.; Wells, B.J.

1985-01-01

A method of bonding elements together with a bond of high strength and good electrical conductivity which comprises: applying an unfilled polyimide resin between surfaces of the elements to be bonded, heat treating said unfilled polyimide resin in stages between a temperature range of about 40 to 365/sup 0/C to form a strong adhesive bond between said elements, applying a metal-filled polyimide resin overcoat between said elements so as to provide electrical connection therebetween, and heat treating said metal-filled polyimide resin with substantially the same temperature profile as the unfilled polyimide resin. The present invention is also concerned with an adhesive, resilient, substantially void free bonding combination for providing a high strength, electrically conductive adhesive attachment between electrically conductive elements which comprises a major amount of an unfilled polyimide resin and a minor amount of a metal-filled polyimide resin.

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.

Electrically conductive resinous bond and method of manufacture

DOEpatents

Snowden, Jr., Thomas M.; Wells, Barbara J.

1987-01-01

A method of bonding elements together with a bond of high strength and good electrical conductivity which comprises: applying an unfilled polyimide resin between surfaces of the elements to be bonded, heat treating said unfilled polyimide resin in stages between a temperature range of about 40.degree. to 365.degree. C. to form a strong adhesive bond between said elements, applying a metal-filled polyimide resin overcoat between said elements so as to provide electrical connection therebetween, and heat treating said metal-filled polyimide resin with substantially the same temperature profile as the unfilled polyimide resin. The present invention is also concerned with an adhesive, resilient, substantially void free bonding combination for providing a high strength, electrically conductive adhesive attachment between electrically conductive elements which comprises a major amount of an unfilled polyimide resin and a minor amount of a metal-filled polyimide resin.

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.

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.

Synthesis and electronic structure determination of N-alkyl-substituted bis(imino)pyridine iron imides exhibiting spin crossover behavior.

PubMed

Bowman, Amanda C; Milsmann, Carsten; Bill, Eckhard; Turner, Zoë R; Lobkovsky, Emil; DeBeer, Serena; Wieghardt, Karl; Chirik, Paul J

2011-11-02

Three new N-alkyl substituted bis(imino)pyridine iron imide complexes, ((iPr)PDI)FeNR ((iPr)PDI = 2,6-(2,6-(i)Pr(2)-C(6)H(3)-N═CMe)(2)C(5)H(3)N; R = 1-adamantyl ((1)Ad), cyclooctyl ((Cy)Oct), and 2-adamantyl ((2)Ad)) were synthesized by addition of the appropriate alkyl azide to the iron bis(dinitrogen) complex, ((iPr)PDI)Fe(N(2))(2). SQUID magnetic measurements on the isomeric iron imides, ((iPr)PDI)FeN(1)Ad and ((iPr)PDI)FeN(2)Ad, established spin crossover behavior with the latter example having a more complete spin transition in the experimentally accessible temperature range. X-ray diffraction on all three alkyl-substituted bis(imino)pyridine iron imides established essentially planar compounds with relatively short Fe-N(imide) bond lengths and two-electron reduction of the redox-active bis(imino)pyridine chelate. Zero- and applied-field Mössbauer spectroscopic measurements indicate diamagnetic ground states at cryogenic temperatures and established low isomer shifts consistent with highly covalent molecules. For ((iPr)PDI)FeN(2)Ad, Mössbauer spectroscopy also supports spin crossover behavior and allowed extraction of thermodynamic parameters for the S = 0 to S = 1 transition. X-ray absorption spectroscopy and computational studies were also performed to explore the electronic structure of the bis(imino)pyridine alkyl-substituted imides. An electronic structure description with a low spin ferric center (S = 1/2) antiferromagnetically coupled to an imidyl radical (S(imide) = 1/2) and a closed-shell, dianionic bis(imino)pyridine chelate (S(PDI) = 0) is favored for the S = 0 state. An iron-centered spin transition to an intermediate spin ferric ion (S(Fe) = 3/2) accounts for the S = 1 state observed at higher temperatures. Other possibilities based on the computational and experimental data are also evaluated and compared to the electronic structure of the bis(imino)pyridine iron N-aryl imide counterparts.

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.

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.

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.

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.

“Thermal Stabilization Effect” of Al2O3 nano-dopants improves the high-temperature dielectric performance of polyimide

PubMed Central

Yang, Yang; He, Jinliang; Wu, Guangning; Hu, Jun

2015-01-01

Insulation performance of the dielectrics under extreme conditions always attracts widespread attention in electrical and electronic field. How to improve the high-temperature dielectric properties of insulation materials is one of the key issues in insulation system design of electrical devices. This paper studies the temperature-dependent corona resistance of polyimide (PI)/Al2O3 nanocomposite films under high-frequency square-wave pulse conditions. Extended corona resistant lifetime under high-temperature conditions is experimentally observed in the 2 wt% nanocomposite samples. The “thermal stabilization effect” is proposed to explain this phenomenon which attributes to a new kind of trap band caused by nanoparticles. This effect brings about superior space charge characteristics and corona resistance under high temperature with certain nano-doping concentration. The proposed theory is experimentally demonstrated by space charge analysis and thermally stimulated current (TSC) tests. This discovered effect is of profound significance on improving high-temperature dielectric properties of nanocomposites towards various applications. PMID:26597981

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.

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.

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

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.

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.

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.

Central neurotoxicity of immunomodulatory drugs in multiple myeloma.

PubMed

Patel, Urmeel H; Mir, Muhammad A; Sivik, Jeffrey K; Raheja, Divisha; Pandey, Manoj K; Talamo, Giampaolo

2015-02-24

Immunomodulatory drugs (IMiDs) currently used in the treatment of multiple myeloma, are thalidomide, lenalidomide and pomalidomide. One of the most common side effects of thalidomide is neurotoxicity, predominantly in the form of peripheral neuropathy. We report 6 cases of significant central neurotoxicity associated with IMiD therapy. Treatment with thalidomide (1 patient), lenalidomide (4 patients), and pomalidomide (1 patient) was associated with various clinical manifestations of central neurotoxicity, including reversible coma, amnesia, expressive aphasia, and dysarthria. Central neurotoxicity should be recognized as an important side effect of IMiD therapy.

Central Neurotoxicity of Immunomodulatory Drugs in Multiple Myeloma

PubMed Central

Patel, Urmeel H.; Mir, Muhammad A.; Sivik, Jeffrey K.; Raheja, Divisha; Pandey, Manoj K.; Talamo, Giampaolo

2015-01-01

Immunomodulatory drugs (IMiDs) currently used in the treatment of multiple myeloma, are thalidomide, lenalidomide and pomalidomide. One of the most common side effects of thalidomide is neurotoxicity, predominantly in the form of peripheral neuropathy. We report 6 cases of significant central neurotoxicity associated with IMiD therapy. Treatment with thalidomide (1 patient), lenalidomide (4 patients), and pomalidomide (1 patient) was associated with various clinical manifestations of central neurotoxicity, including reversible coma, amnesia, expressive aphasia, and dysarthria. Central neurotoxicity should be recognized as an important side effect of IMiD therapy. PMID:25852850

New organic semiconductors with imide/amide-containing molecular systems.

PubMed

Liu, Zitong; Zhang, Guanxin; Cai, Zhengxu; Chen, Xin; Luo, Hewei; Li, Yonghai; Wang, Jianguo; Zhang, Deqing

2014-10-29

Due to their high electron affinities, chemical and thermal stabilities, π-conjugated molecules with imide/amide frameworks have received considerable attentions as promising candidates for high-performance optoelectronic materials, particularly for organic semiconductors with high carrier mobilities. The purpose of this Research News is to give an overview of recent advances in development of high performance imide/amide based organic semiconductors for field-effect transistors. It covers naphthalene diimide-, perylene diimide- and amide-based conjugated molecules and polymers for organic semiconductors. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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.

[Clinical and economic analysis of an internal medicine-infectious disease department at a university general hospital (2005-2006)].

PubMed

Gómez, Joaquín; García-Vázquez, Elisa; Antonio Puertas, José; Ródenas, Julio; Herrero, José Antonio; Albaladejo, Carmen; Baños, Víctor; Canteras, Manuel; Alcaraz, Manolo

2009-02-01

Comparative study in patients with infectious diseases admitted to a specialized Internal Medicine-Infectious Diseases Department (IMID) versus those admitted to other medical departments in a university general hospital, investigating quality and cost-effectiveness. Analysis of patients in 10 principle diagnosis-related groups (DRGs) of infectious diseases admitted to the IMID were compared to those admitted to other medical departments (2005-2006). The DRG were divided in 4 main groups: respiratory infections (DGR 88, 89, 90, 540), urinary infections (DRG 320, 321), sepsis (DRG 416, 584), and skin infections (DRG 277, 278). For each group, quality variables (mortality and readmission rate), efficacy variables (mean hospital stay and mean DRG-based cost per patient) and complexity variables (case mix, relative weight, and functional index) were analyzed. 542 patients included in the 10 main infectious disease DRGs were admitted to IMID and 2404 to other medical departments. After adjusting for DRG case mix (case mix 0.99 for IMID and 0.89 for others), mean hospital stay (5.11 days vs. 7.65 days), mortality (3.5% vs. 7.9%) and mean DRG-based economic cost per patient (1521euro/patient vs. 2952euro/patient) was significantly lower in the group of patients hospitalized in IMID than the group in other medical departments (p<0.05). The readmission rate was similar in the 2 groups (5.5% and 6.5%, respectively). The results per each DRG group were similar to the overall results. For a similar case mix, hospitalization in IMID departments had a positive influence on the variables analyzed as compared to hospitalization in other departments, with a shorter mean stay, lower mortality, and lower mean DRG-based economic cost per patient. Creation and development of IMID departments should be an essential objective to improve healthcare quality and respond to social demands.

Synthesis of temperature and solvent-resistant polymers

NASA Technical Reports Server (NTRS)

Webster, J. A.; Patterson, W. J.; Moffett, R. L.; Morris, D. E.

1972-01-01

Development of silicone polymers, polyimides, and polyisocyanurates for use as insulation, coatings, or adhesives under adverse environmental conditions is discussed. Chemical structure of the organic compounds is presented. Physical and mechanical properties of the compounds are analyzed.

Effect of Nanofiller Characteristics on Nanocomposite Properties

NASA Technical Reports Server (NTRS)

Working, Dennis C.; Lillehei, Peter T.; Lowther, Sharon E.; Siochi, Emilie J.; Kim, Jae-Woo; Sauti, Godfrey; Wise, Kristopher E.; Park, Cheol

2016-01-01

This report surveys the effect of nanofiller characteristics on nanocomposites fabricated with two polyimide matrices. Mechanical and electrical properties were determined. Microscopy results showed that matrix chemistry, nanofiller characteristics and processing conditions had significant impact on nanocomposite quality.

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.

Poly(Amide-imide) Aerogel Materials Produced via an Ice Templating Process

PubMed Central

Gawryla, Matthew D.; Arndt, Eric M.

2018-01-01

Low density composites of sodium montmorillonite and poly(amide-imide) polymers have been created using an ice templating method, which serves as an alternative to the often-difficult foaming of high temperature/high performance polymers. The starting polymer was received in the poly(amic acid) form which can be cured using heat, into a water insoluble amide-imide copolymer. The resulting materials have densities in the 0.05 g/cm3 range and have excellent mechanical properties. Using a tertiary amine as a processing aid provides for lower viscosity and allows more concentrated polymer solutions to be used. The concentration of the amine relative to the acid groups on the polymer backbone has been found to cause significant difference in the mechanical properties of the dried materials. The synthesis and characterization of low density versions of two poly(amide-imide) polymers and their composites with sodium montmorillonite clay are discussed in the present work. PMID:29401663

Poly(Amide-imide) Aerogel Materials Produced via an Ice Templating Process.

PubMed

Gawryla, Matthew D; Arndt, Eric M; Sánchez-Soto, Miguel; Schiraldi, David A

2018-02-03

Low density composites of sodium montmorillonite and poly(amide-imide) polymers have been created using an ice templating method, which serves as an alternative to the often-difficult foaming of high temperature/high performance polymers. The starting polymer was received in the poly(amic acid) form which can be cured using heat, into a water insoluble amide-imide copolymer. The resulting materials have densities in the 0.05 g/cm³ range and have excellent mechanical properties. Using a tertiary amine as a processing aid provides for lower viscosity and allows more concentrated polymer solutions to be used. The concentration of the amine relative to the acid groups on the polymer backbone has been found to cause significant difference in the mechanical properties of the dried materials. The synthesis and characterization of low density versions of two poly(amide-imide) polymers and their composites with sodium montmorillonite clay are discussed in the present work.

Synthesis, Characterization, Topographical Modification, and Surface Properties of Copoly(Imide Siloxane)s

NASA Technical Reports Server (NTRS)

Wohl, Christopher J.; Atkins, Brad M.; Belcher, Marcus A.; Connell, John W.

2012-01-01

Novel copoly(imide siloxane)s were synthesized from commercially available aminopropyl terminated siloxane oligomers, aromatic dianhydrides, and diamines. This synthetic approach produced copolymers with well-defined siloxane blocks linked with imide units in a random fashion. The copoly(amide acid)s were characterized by solution viscosity and subsequently used to cast thin films followed by thermal imidization in an inert atmosphere. Thin films were characterized using contact angle goniometry, attenuated total reflection Fourier transform infrared spectroscopy, confocal and optical microscopy, and tensile testing. Adhesion of micronsized particles was determined quantitatively using a sonication device. The polydimethylsiloxane (PDMS) moieties lowered the copolymer surface energy due to migration of siloxane moieties to the film s surface, resulting in a notable reduction in particle adhesion. A further reduction in particle adhesion was achieved by introducing topographical features on a scale of several to tens of microns by a laser ablation technique.

Design, synthesis, and evaluation of cyclic amide/imide-bearing hydroxamic acid derivatives as class-selective histone deacetylase (HDAC) inhibitors.

PubMed

Shinji, Chihiro; Maeda, Satoko; Imai, Keisuke; Yoshida, Minoru; Hashimoto, Yuichi; Miyachi, Hiroyuki

2006-11-15

A series of hydroxamic acid derivatives bearing a cyclic amide/imide group as a linker and/or cap structure, prepared during our structural development studies based on thalidomide, showed class-selective potent histone deacetylase (HDAC)-inhibitory activity. Structure-activity relationship studies indicated that the steric character of the substituent introduced at the cyclic amide/imide nitrogen atom, the presence of the amide/imide carbonyl group, the hydroxamic acid structure, the shape of the linking group, and the distance between the zinc-binding hydroxamic acid group and the cap structure are all important for HDAC-inhibitory activity and class selectivity. A representative compound (30w) showed potent p21 promoter activity, comparable with that of trichostatin A (TSA), and its cytostatic activity against cells of the human prostate cell line LNCaP was more potent than that of the well-known HDAC inhibitor, suberoylanilide hydroxamic acid (SAHA).

Direct Electrodeposition of UO2 from Uranyl Bis(trifluoromethanesulfonyl)imide Dissolved in 1-Ethyl-3-methylimidazolium Bis(trifluoromethanesulfonyl)imide Room Temperature Ionic Liquid System

DOE PAGES

Freiderich, John W.; Wanigasekara, Eranda P.; Sun, Xiao-Guang; ...

2013-11-11

Our study demonstrates a direct electrodeposition of UO 2 at a Pt cathode from a solution of uranyl bis(trifluoromethanesulfonyl)imide [UO 2(NTf 2) 2)] in a bulk room-temperature ionic liquid (RTIL), 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide (EMIM +NTf 2 –). Cyclic voltammetry (CV) studies revealed two reduction waves corresponding to the conversion of uranium(VI) to uranium(IV), and a mechanism for the overall electroreduction is proposed. A controlled-potential experiment was performed, holding the reduction potential at–1.0 V for 24 h to obtain a brown-black deposit of UO 2 on the Pt cathode. The Faradaic efficiency of the reduction process was determined to be >80%. Themore » UO 2deposit was characterized by powder X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS).« less

Automated Tow Placed LaRC(TM)-PETI-5 Composites

NASA Technical Reports Server (NTRS)

Hou, T. H.; Belvin, H. L.; Johnston, N. J.

2001-01-01

LaRC(TM)-PETI-5 is a PhenylEthynyl-Terminated Imide resin developed at NASA Langley Research Center (LaRC) during the 1990s. It offers a combination of attractive composite and adhesive properties. IM7/LaRC(TM)-PETI-5 composites exhibit thermal and thermo-oxidative stability typical of polyimides, superior chemical resistance and processability, excellent mechanical properties, toughness and damage tolerance. It was selected for study in the High Speed Research program aimed at developing technologies for a future supersonic aircraft, the High Speed Civil Transport, with a projected life span of 60 000 h at a cruise speed up to Mach 2.4. Robust autoclave processing cycles for LaRC(TM)-PETI-5 composites have been thoroughly designed and demonstrated, which involved hand lay-up of solvent-ladened 'wet' prepregs. However, this type of processing is not only costly but also environmentally unfriendly. Volatile management and shrinkage could become serious problems in the fabrication of large complex airframe structural subcomponents. Robotic tow placement technology utilizing 'dry' material forms represents a new fabrication process which overcomes these deficiencies. This work evaluates and compares mechanical properties of composites fabricated by heated head automated tow placement (dry process) with those obtained by hand lay-up/autoclave fabrication (wet process). Thermal and rheological properties of the robotically as-placed uncured composites were measured. A post-cure cycle was designed due to the requirement of the PETI-5 resin for a 370 C/1 h hold to reach full cure, conditions which cannot be duplicated during heated head robotic placement. Mechanical properties such as 0 degree flexural strength and modulus, open hole tensile and compressive strength and moduli, reduced section compression dogbone compressive strength, and modified zippora-medium small (MZ-MS) tensile and compressive properties were obtained on the post-cured panels. These properties compared favourably with those obtained from the wet process.

Wholly Aromatic Ether-imides. Potential Materials for n-Type Semiconductors

NASA Technical Reports Server (NTRS)

Dingemans, Theo J.; St.Clair, Terry L.; Samulski, Edward T.; Bushnell, Dennis M. (Technical Monitor)

2002-01-01

We report on the synthesis and characterization of a novel series low-molar-mass ether-imide rod-shaped model compounds. All ether-imides were obtained by terminating the appropriate rigid core dianhydride, i.e. pyromellitic dianhydride (PMDA), 1,4,5,8-naphthalenetetracarboxylic dianhydride (NDA), 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA), and 3,3,4,4'-oxydiphthalic dianhydride (ODPA) with three flexible aryl-ether tails of different chain length. The mono-functional aryl-ether amines, i.e. 4-(3-phenoxy-phenoxy)-phenylamine (2) and 4-(3-phenoxy-3-phenoxy-phenoxy)-phenylamine (4), were synthesized using standard fluoro-displacement and Ullmann condensation techniques. The corresponding ether-imide model compounds were obtained in high yields using a one-step solution imidization procedure. Increasing the number of meta-substituted aryl-ether units reduces the melt transition temperatures and at the same time it increases the solubility of the model compounds. Most model compounds are crystalline solids and form isotropic melts upon heating. 2,7-Bis-(-4-phenoxy-phenyl)-benzo[Imn][3,8]phenanthroline1,3,6,8-tetraone (NDA-n0), however, displays a smectic A (SA) when cooled from the isotropic phase, followed by what appears to be either a highly ordered smectic phase or a, columnar phase. This is the first example, known to date, in which a mesophase is detected in a wholly aromatic ether-imide compound. For all compounds we present spectroscopic data and X-ray diffraction data. Cyclic voltammetry was used to determine the redox behavior and pertinent energy levels of the model compounds.

PMR-15 polyimide modifications for improved prepreg tack

NASA Technical Reports Server (NTRS)

Vannucci, R. D.

1982-01-01

The use of mixed solvents and of modified monomeric ester reactants was investigated as a means of improving the tack and drape retention characteristics of PMR-15 polyimide prepreg. Methanol, ethanol, 1-propanol and 1-butanol were used to prepare the esters, prepreg solutions, and T-300 graphite fabric and Celion 6000 unidirectional fiber prepregs. The tack retention characteristics of the T-300 fabric prepreg after exposure to simulated use conditions were determined using a simple lap shear test. Drape was qualitatively assessed by visually monitoring the deformability of the prepreg. Thermo-oxidative stability and mechanical properties retention of the Celion 6000 grahite fiber composites were determined as a function of exposure time in air at 600 F.

Transport limited interfacial carrier relaxation in a double-layer device investigated by time-resolved second harmonic generation and impedance spectroscopy

NASA Astrophysics Data System (ADS)

Zhang, Le; Taguchi, Dai; Li, Jun; Manaka, Takaaki; Iwamoto, Mitsumasa

2011-02-01

The interfacial carrier relaxation in an indium tin oxide/polyimide/pentacene/Au double-layer device was studied in both time and frequency domains by using time-resolved second harmonic generation (TR-SHG) and impedance spectroscopy (IS), respectively. Although both hole and electron injection into the pentacene layer and their accumulation at the pentacene/polyimide interface were revealed in TR-SHG, it was only observed in IS under the hole injection condition. The "contradiction" between the two methods for the same carrier relaxation process was explained on the basis of a model, transport limited interfacial carrier relaxation, in which the quasistatic state governs the one-directional carrier transport.

Synthesis and characterization of processable polyimides with enhanced thermal stability

NASA Technical Reports Server (NTRS)

Harris, Frank W.

1987-01-01

Many of the emerging applications of polymers on space vehicles require materials with outstanding thermal stability. These polymers must also be readily processable in order to facilitate their use. The syntheses and polymerization of a cardo dianhydride were investigated. This monomer was prepared via the reaction of N-methyl 4-nitrophthalimide with a cardo diol. Polyimides containing oxyalkylene linkages were studied. The effects of two additional structural modifications on the polymers' properties were investigated. The effects of carrying out the preparation of poly(amic acid)s under non-equilibrium conditions were examined. Approaches that were investigated included the in-situ neutralization of the generated amic acid and its in-situ esterification.

Characterization of thermoplastic polyimide NEW-TPI

NASA Technical Reports Server (NTRS)

Hou, T. H.; Reddy, R. M.

1991-01-01

Thermal and rheological properties of a commercial thermoplastic polyimide, NEW-TPI, were characterized. The as-received material possesses initially a transient crystallite form with a bimodal distribution in peak melting temperatures. After the meltings of the initial crystallite structures, the sample can be recrystallized by various thermal treatments. A bimodal or single-modal melting peak distribution is formed for annealing temperatures below or above 360 C, respectively. The recrystallized crystallinities are all transient in nature. The polymers are unable to be recrystallized after being subjected to elevated temperature annealing above 450 C. The recrystallization mechanism was postulated, and a simple kinetics model was found to describe the behavior satisfactorily under conditions of prolonged thermal annealing.

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.

Thermosetting Phthalocyanine Polymers

NASA Technical Reports Server (NTRS)

Fohlen, G.; Parker, J.; Achar, B.

1985-01-01

Group of phthalocyanine polymers resist thermal degradation. Polymers expected semiconducting. Principal applications probably in molded or laminated parts that have to withstand high temperatures. Polymers made from either of two classes of monomer: Bisphthalonitriles with imide linkages or Bisphthalonitriles with ester-imide linkages.

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.

Novel therapies for immune-mediated inflammatory diseases: What can we learn from their use in rheumatoid arthritis, spondyloarthritis, systemic lupus erythematosus, psoriasis, Crohn's disease and ulcerative colitis?

PubMed

Baker, Kenneth F; Isaacs, John D

2018-02-01

The past three decades have witnessed remarkable advances in our ability to target specific elements of the immune and inflammatory response, fuelled by advances in both biotechnology and disease knowledge. As well as providing superior treatments for immune-mediated inflammatory diseases (IMIDs), such therapies also offer unrivalled opportunities to study the underlying immunopathological basis of these conditions.In this review, we explore recent approaches to the treatment of IMIDs and the insights to pathobiology that they provide. We review novel biologic agents targeting the T-helper 17 axis, including therapies directed towards interleukin (IL)-17 (secukinumab, ixekizumab, bimekizumab), IL-17R (brodalumab), IL-12/23p40 (ustekinumab, briakinumab) and IL-23p19 (guselkumab, tildrakizumab, brazikumab, risankizumab, mirikizumab). We also present an overview of biologics active against type I and II interferons, including sifalumumab, rontalizumab, anifrolumab and fontolizumab. Emerging strategies to interfere with cellular adhesion processes involved in lymphocyte recruitment are discussed, including both integrin blockade (natalizumab, vedolizumab, etrolizumab) and sphingosine-1-phosphate receptor inhibition (fingolimod, ozanimod). We summarise the development and recent application of Janus kinase (JAK) inhibitors in the treatment of IMIDs, including first-generation pan-JAK inhibitors (tofacitinib, baricitinib, ruxolitinib, peficitinib) and second-generation selective JAK inhibitors (decernotinib, filgotinib, upadacitinib). New biologics targeting B-cells (including ocrelizumab, veltuzumab, tabalumab and atacicept) and the development of novel strategies for regulatory T-cell modulation (including low-dose IL-2 therapy and Tregitopes) are also discussed. Finally, we explore recent biotechnological advances such as the development of bispecific antibodies (ABT-122, COVA322), and their application to the treatment of IMIDs. © Article author(s) (or their employer(s) unless otherwise stated in the text of the article) 2018. All rights reserved. No commercial use is permitted unless otherwise expressly granted.

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.

Phosphorus-containing imide resins

NASA Technical Reports Server (NTRS)

Varma, I. K.; Fohlen, G. M.; Parker, J. A. (Inventor)

1985-01-01

Cured polymers of bis and tris-imides derived from tris(m-aminophenyl) phosphine oxides by reaction with maleic anhydride or its derivatives, and addition polymers of such imides, including a variant in which a monoimide is condensed with a dianhydride and the product is treated with a further quantity of maleic anhydride prior to curing are disclosed and claimed. Such polymers are flame resistant. Also disclosed are an improved method of producing tris(m-aminophenyl) phosphine oxides from the nitro analogues by reduction with hydrazine hydrate using palladized charcoal or Raney nickel as the catalyst and fiber reinforced cured resin composites.

Dispersion polymerization of L-lactide utilizing ionic liquids as reaction medium

NASA Astrophysics Data System (ADS)

Fahmiati, Sri; Minami, Hideto; Haryono, Agus; Adilina, Indri B.

2017-11-01

Dispersion polymerization of L-lactide was proceeded in various ionic liquids. Ionic liquids as 1-Hexyl-3-methylimidazolium bis (trifluormethylsulfonyl) imide, [HMIM] [TFSI], 1-Butyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide, [BMP] [TFSI], and N,N,N-Trimethyl-N-Propylammonium Bis (trifloromethanesulfonyl) imide, [TMPA] [TFSI], were employed as reaction medium that dissolved both of lactide and stabilizer (polyvinylprrolidone). Sn-supported on bentonite was used as a ring opening catalyst of L-lactide. Gel Permeation Chromatography result showed that poly-(L-lactic acid) were formed in ionic liquids [HMIM] [TFSI] and [BMP] [TFSI] with molecular weight as 19390 and 20844, respectively.

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 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.

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.

Selective α-arylation of α,β-unsaturated imides mediated by a visible light photoredox catalyst.

PubMed

Ando, Yuki; Kamatsuka, Takuto; Shinokubo, Hiroshi; Miyake, Yoshihiro

2017-08-10

Visible light-mediated α-arylation of α,β-unsaturated imides is achieved via aminium radicals generated from diarylalkylamines using a photoredox catalyst. On the basis of emission quenching experiments, a plausible pathway of the reaction is discussed.

Solvent extraction separation of Th-227 and Ac-225 in room temperature ionic liquids

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

Bell, Jason R; Boll, Rose Ann; Dai, Sheng

2012-01-01

The solvent extractions of Th-227 and Ac-225 from the aqueous phase into ionic liquids (ILs) were investigated by using N,N,N ,N - tetraoctyldiglycolamide (TODGA) or di(2-ethylhexyl)phosphoric acid (HDEHP) as an extractant. Four ionic liquids, 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide ([C4mim][NTf2]), 1-butyl-3-methylimidazolium bis(perfluoroethanesulfonyl)imide ([C4mim][BETI]), 1-butyl-2,3-trimethyleneimidazolium (trifluoromethanesulfonyl)imide [BuI5][NTf2], and 1-benzyl pyridinium bis(trifluoromethanesulfonyl)imide ([PhCH2Py][NTf2]) were used as extraction solvents for separation of Th-227 and Ac-225 in this study. Excellent extraction efficiencies and selectivities were found for Th-227/Ac-225 when HDEHP was used as an extractant in these ionic liquids. The effects of different extractant concentrations in ionic liquids and acidities of the aqueous phase on extraction efficienciesmore » and selectivities of Th-227/Ac-225 are also presented in this article.« less

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.

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.

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.

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.

New Polyimide Has Many Uses

NASA Technical Reports Server (NTRS)

St. Clair, Terry L.; Progar, Donald J.; Smith, Janice Y.; Smith, Ricky E.

1991-01-01

Low-toxicity and low-mutogenicity monomer key to new high-performance polyimide. LaRC-IA is thermoplastic polyimide made from 3-4'-oxydianiline and 4,4'-oxydiphthalic anhydride. Good processing characteristics, low toxicity, and no mutagenicity. Adhesives, composite matrix resins, heat resin moldings, and coating films made of new polymer found to exhibit properties identical or superior to commercially available polyimides. Potential applications wide ranging. With and without end capping, employed to prepare unfilled moldings, coatings and free films, adhesive tape, adhesively bonded substrates, prepregs, and composites.

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 film wear: Effect of temperature and atmosphere

NASA Technical Reports Server (NTRS)

Fusaro, R. L.

1976-01-01

Friction and wear experiments conducted on polyimide films bonded to 440C stainless steel disks indicated that a wear transition (from high wear to low wear) accompanied a friction transition (from high friction to low friction). In dry argon or dry air (less than 20 ppm H2O), the transition was found to occur at 40 plus or minus 10 C; when H20 was present in air (10,000 ppm H2O), the transition was found to be elevated to a temperature between 100 and 200 C. Wear rate calculations made at 25, 100, and 200 C indicated that film wear was relatively constant for particular experimental conditions; however, the rate was strongly dependent on temperature and atmosphere.

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.

Promoting Retention through the Implementation of Integrated Multicultural Instructional Design

ERIC Educational Resources Information Center

Higbee, Jeanne L.; Goff, Emily; Schultz, Jennifer L.

2013-01-01

This article introduces the guiding principles of integrated multicultural instructional design (IMID), a new pedagogical model created to promote retention by addressing multicultural perspectives and social justice issues across the curriculum. To illustrate the model, specific strategies for implementing IMID in a content-based,…

An Efficient Synthesis of de novo Imidates via Aza-Claisen Rearrangements of N-Allyl Ynamides

PubMed Central

DeKorver, Kyle A.; North, Troy D.; Hsung, Richard P.

2010-01-01

A novel thermal 3-aza-Claisen rearrangement of N-allyl ynamides for the synthesis of α-allyl imidates is described. Also, a sequential aza-Claisen, Pd-catalyzed Overman rearrangement is described for the synthesis of azapine-2-ones. PMID:21278848

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.

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.

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.

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.

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.

Thermochemical Properties of the 1-Ethyl-3-Methylimidazolium Bis(trifluoromethylsulfonyl)imide Ionic Liquid under Conditions of Equilibrium with Atmospheric Moisture

NASA Astrophysics Data System (ADS)

Ramenskaya, L. M.; Grishina, E. P.; Kudryakova, N. O.

2018-01-01

Thermochemical properties of the 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl) imide ionic liquid [EMim]NTf2 containing moisture absorbed from the atmosphere (0.242 wt %) are investigated. The phase behavior and thermal stability relative to salt dried in vacuum are studied by means of thermogravimetry and differential scanning calorimetry at different heating and cooling rates. The glass transition, crystallization, and melting temperatures, the enthalpies of phase transitions, and the changes in heat capacity during the formation of glass are determined. It is established that the absorbed water crystallizes at a temperature of around -40.6°C and has virtually no effect on the thermal stability and phase behavior of the salt. Rapid cooling results in the ionic liquid transitioning into the glass state at -91.7 °C and the formation of three mesophases with different melting temperatures; one crystalline modification that melts at a temperature of -19.3°C forms upon slow cooling.

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 Temperature VARTM of Phenylethynyl Terminated Imides

NASA Technical Reports Server (NTRS)

Ghose, Sayata; Watson, Kent A.; Cano, Roberto J.; Britton, Sean M.; Jensen, Brian J.; Connell, John W.; Herring, Helen M.; Linberry, Quentin J.

2009-01-01

LaRC phenylethynyl terminated imide (PETI) resins were processed into composites using high temperature vacuum assisted resin transfer molding (VARTM). Although initial runs yielded composites with high void content, process modifications reduced voids to <3%. Photomicrographs were taken and void contents and T(sub g)s of the panels were determined.

Nanocrystallization of LiCoO2 Cathodes for Thin Film Batteries Utilizing Pulse Thermal Processing

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

None

2009-04-01

This factsheet describes a study whose focus is on the nanocrystallization of the LiCoO2 cathode thin films on polyimide substrates and evaluate the microstructural evolution and resistance as a function of PTP processing conditions.

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. 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 modified 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. The composites were exposed to a thermal radiation of 5.3 Btu/sq ft-sec in air. Samples of each of the unfilled composite were decomposed anaerobically in the calorimeter. Weight loss data were recorded for burning and decomposition times up to thirty-five minutes. 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 burned in air. Boron powder additions to both the polyimide and the epoxy resins stabilized the chars and effectively controlled the fiber release.

Polyimide surface modification by using microwave plasma for adhesion enhancement of Cu electroless plating.

PubMed

Cho, Sang-Jin; Nguyen, Trieu; Boo, Jin-Hyo

2011-06-01

Microwave (MW) plasma was applied to the surface of polyimide (PI) films as a treatment to enhance the adhesion between copper deposition layer and PI surface for electroless plating. The influences of nitrogen MW plasma treatment on chemical composition of the PI surface were investigated by using X-Ray photoelectron spectroscopy (XPS). The wettability was also investigated by water contact angle measurement. The surface morphologies of PI films before and after treatment were characterized with atomic force microscopy (AFM). The contact angle results show that was dramatically decreased to 16.1 degrees at the optimal treatment condition from 72.1 degrees (untreated PI). However, the root mean square (RMS) roughness of treated PI film was almost unchanged. The AFM roughness was stayed from 1.0 to 1.2 with/without plasma treatment. XPS data show a nitrogen increase when PI films exposed to N2 MW plasma. Electroless copper depositions were carried out with the free-formaldehyde method using glyoxylic acid as the reducing reagent and mixture palladium chloride, tin chloride as activation solution. Adhesion property between polyimide surface and copper layer was investigated by tape test.

Fabrication of nanochannels on polyimide films using dynamic plowing lithography

NASA Astrophysics Data System (ADS)

Stoica, Iuliana; Barzic, Andreea Irina; Hulubei, Camelia

2017-12-01

Three distinct polyimide films were analyzed from the point of view of their morphology in order to determine if their surface features can be adapted for applications where surface anisotropy is mandatory. Channels of nanometric dimensions were created on surface of the specimens by using a less common atomic force microscopy (AFM) method, namely Dynamic Plowing Lithography (DPL). The changes generated by DPL procedure were monitored through the surface texture and other functional parameters, denoting the surface orientation degree and also bearing and fluid retention properties. The results revealed that in the same nanolithography conditions, the diamine and dianhydride moieties have affected the characteristics of the nanochannels. This was explained based on the aliphatic/aromatic nature of the monomers and the backbone flexibility. The reported data are of great importance in designing custom nanostructures with enhanced anisotropy on surface of polyimide films for liquid crystal orientation or guided cell growth purposes. At the end, to track the effect of the nanolithography process on the tip sharpness, degradation and contamination, the blind tip reconstruction was performed on AFM probe, before and after lithography experiments, using TGT1 test grating AFM image.

Synergistic effects of ultraviolet radiation, thermal cycling and atomic oxygen on altered and coated Kapton surfaces

NASA Technical Reports Server (NTRS)

Dever, Joyce A.; Bruckner, Eric J.; Rodriguez, Elvin

1992-01-01

The photovoltaic (PV) power system for Space Station Freedom (SSF) uses solar array blankets which provide structural support for the solar cells and house the electrical interconnections. In the low earth orbital (LEO) environment where SSF will be located, surfaces will be exposed to potentially damaging environmental conditions including solar ultraviolet (UV) radiation, thermal cycling, and atomic oxygen. It is necessary to use ground based tests to determine how these environmental conditions would affect the mass loss and optical properties of candidate SSF blanket materials. Silicone containing, silicone coated, and SiO(x) coated polyimide film materials were exposed to simulated LEO environmental conditions to determine their durability and whether the environmental conditions of UV, thermal cycling and oxygen atoms act synergistically on these materials. A candidate PV blanket material called AOR Kapton, a polysiloxane polyimide cast from a solution mixture, shows an improvement in durability to oxygen atoms erosion after exposure to UV radiation or thermal cycling combined with UV radiation. This may indicate that the environmental conditions react synergistically with this material, and the damage predicted by exposure to atomic oxygen alone is more severe than that which would occur in LEO where atomic oxygen, thermal cycling and UV radiation are present together.

Synergistic effects of ultraviolet radiation, thermal cycling, and atomic oxygen on altered and coated Kapton surfaces

NASA Technical Reports Server (NTRS)

Dever, Joyce A.; Bruckner, Eric J.; Rodriguez, Elvin

1992-01-01

The photovoltaic (PV) power system for Space Station Freedom (SSF) uses solar array blankets which provide structural support for the solar cells and house the electrical interconnections. In the low Earth orbital (LEO) environment where SSF will be located, surfaces will be exposed to potentially damaging environmental conditions including solar ultraviolet (UV) radiation, thermal cycling, and atomic oxygen. It is necessary to use ground based tests to determine how these environmental conditions would affect the mass loss and optical properties of candidate SSF blanket materials. Silicone containing, silicone coated, and SiO(x) coated polyimide film materials were exposed to simulated LEO environmental conditions to determine there durability and whether the environmental conditions of UV, thermal cycling and oxygen atoms act synergistically on these materials. A candidate PV blanket material called AOR Kapton, a polysiloxane polyimide cast from a solution mixture, shows an improvement in durability to oxygen atoms erosion after exposure to UV radiation or thermal cycling combined with UV radiation. This may indicate that the environmental conditions react synergistically with this material, and the damage predicted by exposure to atomic oxygen alone is more severe than that which would occur in LEO where atomic oxygen, thermal cycling and UV radiation are present together.

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.

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.

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.

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.

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.

Corrosion of stainless steel battery components by bis(fluorosulfonyl)imide based ionic liquid electrolytes

NASA Astrophysics Data System (ADS)

Evans, Tyler; Olson, Jarred; Bhat, Vinay; Lee, Se-Hee

2014-12-01

While the anodic behavior of aluminum foil current collectors in imide-based room temperature ionic liquids (RTILs) is relatively well understood, interactions between such RTILs and other passive battery components have not been studied extensively. This study presents the solvent and potential dependent oxidation of SS316 coin-cell components in the N-methyl-N-propyl-pyrrolidinium bis(fluorosulfonyl)imide (PYR13FSI) RTIL. While this phenomenon prohibits high-voltage cycling of Li(Ni1/3Mn1/3Co1/3)O2 cathodes in SS316 coin-type cells, Al-clad cell components or alternative cell configurations can be utilized to avoid SS316 oxidation-induced cell failure.

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.

21 CFR 177.2450 - Polyamide-imide resins.

Code of Federal Regulations, 2010 CFR

2010-04-01

... Determination as set forth in the “Official Methods of Analysis of the Association of Official Analytical... chromatography method titled “Amide-Imide Polymer Analysis—Analysis of Monomer Content,” is incorporated by... of films of 1 mil uniform thickness after coating and heat curing at 600 °F for 15 minutes on...

Immunomodulatory drugs in multiple myeloma: mechanisms of action and clinical experience

PubMed Central

Holstein, Sarah A.; McCarthy, Philip L.

2017-01-01

Over the last two decades, the outcomes for patients with multiple myeloma, a plasma cell malignancy, have dramatically improved. The development of the immunomodulatory drugs (IMiDs) which include thalidomide, lenalidomide, and pomalidomide, has contributed significantly to these improved outcomes. While thalidomide is now less commonly prescribed, lenalidomide is widely used in the treatment of newly diagnosed transplant-eligible and transplant-ineligible patients, in the maintenance setting post-transplant and in the relapsed/refractory setting, while pomalidomide is currently utilized in the relapsed/refractory setting. The IMiDs have been reported to have a multitude of activities, including anti-angiogenic, cytotoxic, and immunomodulatory, however, the more recent discoveries that the IMiDs bind to cereblon and thus regulate the ubiquitination of key transcription factors including IKZF1 and IKZF3, have provided greater insight into their mechanism of action. Here the clinical efficacy of these agents in myeloma is reviewed as well as discussion of structure-function relationship, the molecular mechanisms of action, and the association of IMiDs with second primary malignancies and thrombosis. PMID:28205024

Structure of the DDB1-CRBN E3 ubiquitin ligase in complex with thalidomide

PubMed Central

Fischer, Eric S.; Böhm, Kerstin; Lydeard, John R.; Yang, Haidi; Stadler, Michael B.; Cavadini, Simone; Nagel, Jane; Serluca, Fabrizio; Acker, Vincent; Lingaraju, Gondichatnahalli M.; Tichkule, Ritesh B.; Schebesta, Michael; Forrester, William C.; Schirle, Markus; Hassiepen, Ulrich; Ottl, Johannes; Hild, Marc; Beckwith, Rohan E. J.; Harper, J. Wade; Jenkins, Jeremy L.; Thomä, Nicolas H.

2015-01-01

In the 1950s the drug thalidomide administered as a sedative to pregnant women led to the birth of thousands of children with multiple defects. Despite its teratogenicity, thalidomide and its derivatives lenalidomide and pomalidomide (together known as Immunomodulatory Drugs: IMiDs) recently emerged as effective treatments for multiple myeloma and 5q-dysplasia. IMiDs target the CUL4-RBX1-DDB1-CRBN (CRL4CRBN) E3 ubiquitin ligase and promote the ubiquitination of Ikaros/Aiolos transcription factors by CRL4CRBN. Here we present the crystal structure of the DDB1-CRBN complex bound to thalidomide, lenalidomide and pomalidomide. The structure establishes CRBN as a CRL4CRBN substrate receptor, which enantioselectively binds IMiDs. Through an unbiased screen we identify the homeobox transcription factor MEIS2 as an endogenous substrate of CRL4CRBN. Our studies suggest that IMiDs block endogenous substrates (MEIS2) from binding to CRL4CRBN when recruiting Ikaros/Aiolos for degradation. This dual activity implies that small molecules can principally modulate a ligase to up- or down-regulate the ubiquitination of proteins. PMID:25043012

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.

Composite Properties of Polyimide Resins Made From "Salt-Like" Solution Precursors

NASA Technical Reports Server (NTRS)

Cano, Roberto J.; Weiser, Erik S.; SaintClair, Terry L.; Echigo, Yoshiaki; Kaneshiro, Hisayasu

1997-01-01

Recent work in high temperature materials at NASA Langley Research Center (LaRC (trademark)) have led to the development of new polyimide resin systems with very attractive properties. The majority of the work done with these resin systems has concentrated on determining engineering mechanical properties of composites prepared from a poly(amide acid) precursor. Three NASA Langley-developed polyimide matrix resins, LaRC (trademark) -IA, LaRC (trademark) -IAX, and LaRC (trademark) -8515, were produced via a salt-like process developed by Unitika Ltd. The 'salt-like' solutions (sixty-five percent 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. Mechanical properties are presented for these three intermediate modulus carbon fiber/polyimide matrix composites and compared to existing data on the same polyimide resin systems and IM7 carbon fiber manufactured via poly(amide acid) solutions (thirty-five percent solids in NMP). This work studies the effects of varying the synthetic route on the processing and mechanical properties of polyimide composites.

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.

Imide Oligomers Containing Pendent and Terminal Phenylethynyl Groups-2

NASA Technical Reports Server (NTRS)

Connell, J. W.; Smith, J. G., Jr.; Hergenrother, P. M.

1998-01-01

As part of a program to develop high-performance/high-temperature structural resins for aeronautical applications, imide oligomers containing pendent and terminal phenylethynyl groups were prepared, characterized and the cured resins evaluated as composite matrices. The oligomers were prepared at a calculated number-average molecular weight of 5000 g/mol and contained 15-20 mol% pendent phenylethynyl groups. In previous work, an oligomer containing pendent and terminal phenylethynyl groups exhibited a high glass transition temperature (approximately 313 C), and laminates therefrom exhibited high compressive properties, but processability, fracture toughness, microcrack resistance and damage tolerance were less than desired. In an attempt to improve these deficiencies, modifications in the oligomeric backbone involving the incorporation of 1,3-bis(3-aminophenoxy)benzene were investigated as a means of improving processability and toughness without detracting from the high glass transition temperature and high compressive properties. The amide acid oligomeric solutions were prepared in N-methyl-2-pyrrolidinone and were subsequently processed into imide powder, thin films, adhesive tape and carbon fiber prepreg. Neat resin plaques were fabricated from imide powder by compression moulding. The maximum processing pressure was 1.4 MPa and the cure temperature ranged from 350 to 371 C for 1 h for the mouldings, adhesives, films and composites. The properties of the 1,3-bis(3-aniinophenoxy)benzene modified cured imide oligomers containing pendent and terminal phenylethynyl groups are compared with those of previously prepared oligomers containing pendent and terminal phenylethynyl groups of similar composition and molecular weight.

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.

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.

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.

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.

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.

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

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.

Photopiezoelectric Composites of Azobenzene-Functionalized Polyimides and Polyvinylidene Fluoride (Postprint)

DTIC Science & Technology

2014-10-01

equilib- rium condition, exposure of the undrawn and drawn azo- BPA -6FDI-100 material to sequenced irradiation at 0.25 Hz generates signifi cant changes...crossed polarizers, showing green birefringence color. c) Photogenerated stress with sequenced light irradia- tion of undrawn and drawn azo- BPA -6FDI-100

Processing of Superconductor-Normal-Superconductor Josephson Edge Junctions

NASA Technical Reports Server (NTRS)

Kleinsasser, A. W.; Barner, J. B.

1997-01-01

The electrical behavior of epitaxial superconductor-normal-superconductor (SNS) Josephson edge junctions is strongly affected by processing conditions. Ex-situ processes, utilizing photoresist and polyimide/photoresist mask layers, are employed for ion milling edges for junctions with Yttrium-Barium-Copper-Oxide (YBCO) electrodes and primarily Co-doped YBCO interlayers.

Preparation of pyrrolizinone derivatives via sequential transformations of cyclic allyl imides: synthesis of quinolactacide and marinamide.

PubMed

Simic, Milena; Tasic, Gordana; Jovanovic, Predrag; Petkovic, Milos; Savic, Vladimir

2018-03-28

A facile synthetic route has been developed for the preparation of pyrrolizinone derivatives employing N-allyl imides as starting materials. The nucleophilic addition of a vinyl Grignard reagent/RCM/elimination sequence afforded pyrrolizinones in good yields and has been applied for the preparation of naturally occurring quinolactacide and marinamide.

Electrochromic Salts, Solutions, and Devices

DOEpatents

Burrell, Anthony K.; Warner, Benjamin P.; McClesky, T. Mark

2008-11-11

Electrochromic salts. Electrochromic salts of dicationic viologens such as methyl viologen and benzyl viologen associated with anions selected from bis(trifluoromethylsulfonyl)imide, bis(perfluoroethylsulfonyl)imide, and tris(trifluoromethylsulfonyl)methide are produced by metathesis with the corresponding viologen dihalide. They are highly soluble in molten quarternary ammonium salts and together with a suitable reductant provide electrolyte solutions that are used in electrochromic windows.

Electrochromic salts, solutions, and devices

DOEpatents

Burrell, Anthony K [Los Alamos, NM; Warner, Benjamin P [Los Alamos, NM; McClesky,7,064,212 T. Mark

2006-06-20

Electrochromic salts. Electrochromic salts of dicationic viologens such as methyl viologen and benzyl viologen associated with anions selected from bis(trifluoromethylsulfonyl)imide, bis(perfluoroethylsulfonyl)imide, and tris(trifluoromethylsulfonyl)methide are produced by metathesis with the corresponding viologen dihalide. They are highly soluble in molten quarternary ammonium salts and together with a suitable reductant provide electrolyte solutions that are used in electrochromic windows.

Electrochromic Salts, Solutions, and Devices

DOEpatents

Burrell, Anthony K.; Warner, Benjamin P.; McClesky, T. Mark

2008-10-14

Electrochromic salts. Electrochromic salts of dicationic viologens such as methyl viologen and benzyl viologen associated with anions selected from bis(trifluoromethylsulfonyl)imide, bis(perfluoroethylsulfonyl)imide, and tris(trifluoromethylsulfonyl)methide are produced by metathesis with the corresponding viologen dihalide. They are highly soluble in molten quarternary ammonium salts and together with a suitable reductant provide electrolyte solutions that are used in electrochromic windows.

Chiral imidate-ferrocenylphosphanes: synthesis and application as P,N-ligands in iridium(I)-catalyzed hydrogenation of unfunctionalized and poorly functionalized olefins.

PubMed

Bert, Katrien; Noël, Timothy; Kimpe, Wim; Goeman, Jan L; Van der Eycken, Johan

2012-11-14

A small library of chiral imidate-ferrocenylphosphane ligands was efficiently synthesized (8 examples) and evaluated in the iridium(I)-catalyzed hydrogenation of unfunctionalized and poorly functionalized olefins. These catalysts perform very well in a range of examples (yields and ee's up to 100%).

Lithium insertion in graphite from ternary ionic liquid-lithium salt electrolytes. I. Electrochemical characterization of the electrolytes

NASA Astrophysics Data System (ADS)

Appetecchi, Giovanni B.; Montanino, Maria; Balducci, Andrea; Lux, Simon F.; Winterb, Martin; Passerini, Stefano

In this paper we report the results of chemical-physical investigation performed on ternary room temperature ionic liquid-lithium salt mixtures as electrolytes for lithium-ion battery systems. The ternary electrolytes were made by mixing N-methyl- N-propyl pyrrolidinium bis(fluorosulfonyl) imide (PYR 13FSI) and N-butyl- N-methylpyrrolidinium bis(trifluoromethanesulfonyl) imide (PYR 14TFSI) ionic liquids with lithium hexafluorophosphate (LiPF 6) or lithium bis(trifluoromethanesulfonyl)imide (LiTFSI). The mixtures were developed based on preliminary results on the cyclability of graphite electrodes in the IL-LiX binary electrolytes. The results clearly show the beneficial synergic effect of the two ionic liquids on the electrochemical properties of the mixtures.

Demonstrating hydrogen production from ammonia using lithium imide - Powering a small proton exchange membrane fuel cell

NASA Astrophysics Data System (ADS)

Hunter, Hazel M. A.; Makepeace, Joshua W.; Wood, Thomas J.; Mylius, O. Simon; Kibble, Mark G.; Nutter, Jamie B.; Jones, Martin O.; David, William I. F.

2016-10-01

Accessing the intrinsic hydrogen content within ammonia, NH3, has the potential to play a very significant role in the future of a CO2-free sustainable energy supply. Inexpensive light metal imides and amides are effective at decomposing ammonia to hydrogen and nitrogen (2NH3 → 3H2 + N2), at modest temperatures, and thus represent a low-cost approach to on-demand hydrogen production. Building upon this discovery, this paper describes the integration of an ammonia cracking unit with a post-reactor gas purification system and a small-scale PEM fuel cell to create a first bench-top demonstrator for the production of hydrogen using light metal imides.

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.

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.

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.

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.

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.

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.

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.

Depolarization current relaxation process of insulating dielectrics after corona poling under different charging conditions

NASA Astrophysics Data System (ADS)

Zhang, J. W.; Zhou, T. C.; Wang, J. X.; Yang, X. F.; Zhu, F.; Tian, L. M.; Liu, R. T.

2017-10-01

As an insulating dielectric, polyimide is favorable for the application of optoelectronics, electrical insulation system in electric power industry, insulating, and packaging materials in space aircraft, due to its excellent thermal, mechanical and electrical insulating stability. The charge storage profile of such insulating dielectric is utmost important to its application, when it is exposed to electron irradiation, high voltage corona discharge or other treatments. These treatments could induce changes in physical and chemical properties of treated samples. To investigate the charge storage mechanism of the insulating dielectrics after high-voltage corona discharge, the relaxation processes responsible for corona charged polyimide films under different poling conditions were analyzed by the Thermally Stimulated Discharge Currents method (TSDC). In the results of thermal relaxation process, the appearance of various peaks in TSDC spectra provided a deep insight into the molecular status in the dielectric material and reflected stored space charge relaxation process in the insulating polymers after corona discharge treatments. Furthermore, the different space charge distribution status under various poling temperature and different discharge voltage level were also investigated, which could partly reflect the influence of the ambiance condition on the functional dielectrics after corona poling.

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.

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.

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.

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.

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.

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.

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.

Conductivity and spectroscopic investigation of bis(trifluoromethanesulfonyl)imide solution in ionic liquid 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide.

PubMed

Yu, Lei; Pizio, Benjamin S; Vaden, Timothy D

2012-06-07

Protic ionic liquids (PILs) are promising alternatives to water for swelling Nafion as a fuel cell proton exchange membrane (PEM). PILs can significantly improve the high-temperature performance of a PEM. The proton dissociation and solvation mechanisms in a PIL, which are keys to understanding the proton transportation and conductivity, have not been fully explored. In this paper, we used FTIR, Raman, and electronic spectroscopy with computational simulation techniques to explore the spectroscopic properties of bis(trifluoromethanesulfonyl)imide (HTFSI) solutions in 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide (BMITFSI) ionic liquid at concentrations from ∼0.1 to as high as ∼1.0 M. Solution conductivities were measured at room temperature and elevated temperatures up to ∼65 °C. The solution structure and properties depend on the concentration of HTFSI. At lower concentration, around 0.1 M, the HTFSI solution has higher conductivity than pure BMITFSI. However, the conductivity decreases when the concentration increases from 0.1 to 1.0 M. Temperature-dependent conductivities followed the Vogel-Fulcher-Tamman equation at all concentrations. Conductivity and spectroscopy results elucidate the complicated ionization and solvation mechanism of HTFSI in BMITFSI solutions. Raman spectroscopy and density functional theory (DFT) calculations are consistent with the complete ionization of HTFSI to generate solvated H(+) at low concentrations. FTIR, Raman, and electronic spectroscopic results as well as DFT computational simulation indicated that when the concentration is as high as 1.0 M, a significant amount of TFSI(-) is protonated, most likely at the imide nitrogen.

Cycling and rate performance of Li-LiFePO 4 cells in mixed FSI-TFSI room temperature ionic liquids

NASA Astrophysics Data System (ADS)

Lewandowski, A. P.; Hollenkamp, A. F.; Donne, S. W.; Best, A. S.

A study is conducted of the performance of lithium iron(II) phosphate, LiFePO 4, as a cathode material in a lithium secondary battery that features an ionic liquid electrolyte solution and a metallic lithium anode. The electrolyte solution comprises an ionic liquid of a N-methyl-N-alkyl-pyrrolidinium (alkyl = n-propyl or n-butyl) cation and either the bis(fluorosulfonyl)imide [(FSO 2) 2N -] or bis(trifluoromethanesulfonyl)imide [(F 3CSO 2) 2N -] anion, together with 0.5 mol kg -1 of lithium bis(trifluoromethanesulfonyl)imide salt. For N-methyl-N-propyl-pyrrolidinium bis(fluorosulfonyl)imide, coin cells discharging at rates of C/10 and 4C yield specific capacities of 153 and 110 mAh g -1, respectively, at an average coulombic efficiency of 99.8%. This performance is maintained for over 400 cycles at 50 °C and therefore indicates that these electrolyte solutions support long-term cycling of both LiFePO 4 and metallic lithium while, due to the negligible volatility of ionic liquids, surrounding the lithium in an inherently safe, non-flammable medium.

Molecular dynamics simulations of trans- and cis- N-acetyl- N'-methylamides of XaaPro dipeptides

NASA Astrophysics Data System (ADS)

Hoon Choi, Seung; Yun Yu, Jeong; Kwang Shin, Jae; Shik Jhon, Mu

1994-07-01

The occurrence of cis imide bonds in proteins is much higher than that of cis amide bonds due to the unique properties of proline. In order to examine the relationship between the high occurrence of these cis imide bonds and the residues preceding the proline, we perform molecular dynamics simulations of trans- and cis- N-acetyl- N'-methylamides of XaaPro dipeptides (AcXaaProNHMe). We investigate the conformational energies and structures of trans- and cis-AcXaa where Xaa has 12 amino acids in the vacuum state and 5 amino acids in the solution state. It is found that the occurrence of the cis imide bonds is strongly affected by the residue preceding the proline, and the dihedral angles (φ,ψ) of the backbone in AcXaaProNHMe are influenced by the configuration of the imide bond. We also find that the equilibrium properties of XaaPro in solution simulations are more similar to the statistics of X-ray crystallographic data than are those in vacuum simulations and solvation causes a remarkable change in the conformation of the pyrrolidine ring from the endo to the exo form.

Thermal design of spacecraft solar arrays using a polyimide foam

NASA Astrophysics Data System (ADS)

Bianco, N.; Iasiello, M.; Naso, V.

2015-11-01

The design of the Thermal Control System (TCS) of spacecraft solar arrays plays a fundamental role. Indeed, the spacecraft components must operate within a certain range of temperature. If this doesn't occur, their performance is reduced and they may even break. Solar arrays, which are employed to recharge batteries, are directly exposed to the solar heat flux, and they need to be insulated from the earth's surface irradiation. Insulation is currently provided either with a white paint coating or with a Multi Layer Insulation (MLI) system [1]. A configuration based on an open-cell polyimide foam has also been recently proposed [2]. Using polyimide foams in TCSs looks very attractive in terms of costs, weight and assembling. An innovative thermal analysis of the above cited TCS configurations is carried out in this paper, by solving the porous media energy equation, under the assumption of Local Thermal Equilibrium (LTE) between the two phases. Radiation effects through the solar array are also considered by using the Rosseland approximation. Under a stationary daylight condition, temperature profiles are obtained by means of the finite-element based code COMSOL Multiphysics®. Finally, since the weight plays an important role in aerospace applications, weights of the three TCS configurations are compared.

Synthesis and properties of reprocessable sulfonated polyimides cross-linked via acid stimulation for use as proton exchange membranes

NASA Astrophysics Data System (ADS)

Zhang, Boping; Ni, Jiangpeng; Xiang, Xiongzhi; Wang, Lei; Chen, Yongming

2017-01-01

Cross-linked sulfonated polyimides are one of the most promising materials for proton exchange membrane (PEM) applications. However, these cross-linked membranes are difficult to reprocess because they are insoluble. In this study, a series of cross-linkable sulfonated polyimides with flexible pendant alkyl side chains containing trimethoxysilyl groups is successfully synthesized. The cross-linkable polymers are highly soluble in common solvents and can be used to prepare tough and smooth films. Before the cross-linking reaction is complete, the membranes can be reprocessed, and the recovery rate of the prepared films falls within an acceptable range. The cross-linked membranes are obtained rapidly when the cross-linkable membranes are immersed in an acid solution, yielding a cross-linking density of the gel fraction of greater than 90%. The cross-linked membranes exhibit high proton conductivities and tensile strengths under hydrous conditions. Compared with those of pristine membranes, the oxidative and hydrolytic stabilities of the cross-linked membranes are significantly higher. The CSPI-70 membrane shows considerable power density in a direct methanol fuel cell (DMFC) test. All of these results suggest that the prepared cross-linked membranes have great potential for applications in proton exchange membrane fuel cells.

Reducing Stiffness and Electrical Losses of High Channel Hybrid Nerve Cuff Electrodes

DTIC Science & Technology

2001-10-25

Electrodes were developed. These electrodes consisted of a micromachined polyimide -based thin-film structure with integrated electrode contacts and...electrodes, mechanical properties were enhanced by changing the method of joining silicone and polyimide from using one part silicone adhesive to...gold, platinum, platinum black, polyimide , silicone, polymer bonding I. INTRODUCTION Cuff-type electrodes are probably the most commonly used neural

Viscoelasticity and Creep Recovery of Polyimide Thin Films

DTIC Science & Technology

1990-06-01

3931; (617) 253-0292. Accesion For NTIS CRA&I DTIC TAB Unannounced 0 JuslfIcation .... ’ ry (I’. . ,* VISCOELASTICITY AND CREEP RECOVERY OF POLYIMIDE...polyimide is subjected to sustained loads. Viscoelastic properties of materials are traditionally measured by uniaxial tests [4]. Creep, stress...structure The membrane fabrication and analysis is implemented in the environment of a previously reported CAD architecture [7,81, which uses a

Polyimide-glass multilayer printed wiring boards

NASA Astrophysics Data System (ADS)

Lula, J. W.

1984-07-01

Multilayer printed wiring boards (PWBs) from a polyimide/glass reinforced copper clad laminate and prepreg were manufactured. A lamination cycle and innerlayer copper surface treatment that gave satisfactory delamination resistance at soldering temperatures were developed. When compared to similar epoxy/glass multilayer PWBs, the polyimide PWBs had higher thermal stability, greater resistance to raised lands, fewer plating voids, less outgassing, and adhesion that was equivalent to urethane foam encapsulants.

Thin Films Protect Electronics from Heat and Radiation

NASA Technical Reports Server (NTRS)

2013-01-01

While Anne St. Clair worked on high performance polyimides at Langley Research Center, she noticed that some of the films were nearly colorless. The polyimides became known as LaRC-CP1 and LaRC-CP2, and were licensed by NeXolve Corporation, based in Huntsville, Alabama. Today, NeXolve provides polyimide film products to commercial customers for spacecraft, telescopes, and circuit boards.

Effects of combined irradiation of 500 keV protons and atomic oxygen on polyimide films

NASA Astrophysics Data System (ADS)

Novikov, Lev; Chernik, Vladimir; Zhilyakov, Lev; Voronina, Ekaterina; Chirskaia, Natalia

2016-07-01

Polyimide films are widely used on the spacecraft surface as thermal control coating, films in different constuctions, etc. However, the space ionizing radiation of different types can alter the mechanical, optical and electrical properties of polyimide films. For example, it is well known that 20-100 keV proton irradiation causes breaking of chemical bonds and destruction of the surface layer in polyimide, deterioration of its optical properties, etc. In low-Earth orbits serious danger for polymeric materials is atomic oxygen of the upper atmosphere of the Earth, which is the main component in the range of heights of 200-800 km. Due to the orbital spacecraft velocity, the collision energy of oxygen atoms with the surface ( 5 eV) enhances their reactivity and opens additional pathways of their reaction with near-surface layers of materials. Hyperthermal oxygen atom flow causes erosion of the polyimide surface by breaking chemical bonds and forming of volatiles products (primarily, CO and CO _{2}), which leads to mass losses and degradation of material properties. Combined effect of protons and oxygen plasma is expected to give rise to synergistic effects enhancing the destruction of polyimide surface layers. This paper describes experimental investigation of polyimide films sequential irradiation with protons and oxygen plasma. The samples were irradiated by 500 keV protons at fluences of 10 ^{14}-10 ^{16} cm ^{-2} produced with SINP cascade generator KG-500 and 5-20 eV neutral oxygen atoms at fluence of 10 ^{20} cm ^{-2} generated by SINP magnetoplasmodynamics accelerator. The proton bombardment causes the decrease in optical transmission coefficient of samples, but their transmittance recovers partially after the exposure to oxygen plasma. The results of the comparative analysis of polyimide optical transmission spectra, Raman and XPS spectra obtained at different stages of the irradiation of samples, data on mass loss of samples due to erosion of the surface are given. The report also presents the results of computer simulation of protons and oxygen atoms interaction with polyimide, and a comparison of the experimental and calculated data.

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.

Electroless deposition of Au nanoparticles on reduced graphene oxide/polyimide film for electrochemical detection of hydroquinone and catechol

NASA Astrophysics Data System (ADS)

Shen, Xuan; Xia, Xiaohong; Du, Yongling; Wang, Chunming

2017-09-01

An electrochemical sensor for determination of hydroquinone (HQ) and catechol (CC) was developed using Au nanoparticles (AuNPs) fabricated on reduced graphene oxide/polyimide (PI/RGO) film by electroless deposition. The electrochemical behaviors of HQ and CC at PI/RGO-AuNPs electrode were investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Under the optimized condition, the current responses at PI/RGO-AuNPs electrode were linear over ranges from 1 to 654 mol/L for HQ and from 2 to 1289 mol/L for CC, with the detection limits of 0.09 and 0.2 mol/L, respectively. The proposed electrode exhibited good reproducibility, stability and selectivity. In addition, the proposed electrode was successfully applied in the determination of HQ and CC in tap water and the Yellow River samples.

Fabrication of Polyimide-Matrix/Carbon and Boron-Fiber Tape

NASA Technical Reports Server (NTRS)

Belvin, Harry L.; Cano, Roberto J.; Treasure, Monte; Shahood, Thomas W.

2007-01-01

The term HYCARB denotes a hybrid composite of polyimide matrices reinforced with carbon and boron fibers. HYCARB and an improved process for fabricating dry HYCARB tapes have been invented in a continuing effort to develop lightweight, strong composite materials for aerospace vehicles. Like other composite tapes in this line of development, HYCARB tapes are intended to be used to build up laminated structures having possibly complex shapes by means of automated tow placement (ATP) - a process in which a computer-controlled multiaxis machine lays down prepreg tape or tows. The special significance of the present process for making dry HYCARB for ATP is that it contributes to the reduction of the overall cost of manufacturing boron-reinforced composite-material structures while making it possible to realize increased compression strengths. The present process for making HYCARB tapes incorporates a "wet to dry" process developed previously at Langley Research Center. In the "wet to dry" process, a flattened bundle of carbon fiber tows, pulled along a continuous production line between pairs of rollers, is impregnated with a solution of a poly(amide acid) in N-methyl-2-pyrrolidinone (NMP), then most of the NMP is removed by evaporation in hot air. In the present case, the polyamide acid is, more specifically, that of LaRC. IAX (or equivalent) thermoplastic polyimide, and the fibers are, more specifically, Manganite IM7 (or equivalent) polyacrylonitrile- based carbon filaments that have a diameter of 5.2 m and are supplied in 12,000-filament tows. The present process stands in contrast to a prior process in which HYCARB tape was made by pressing boron fibers into the face of a wet carbon-fiber/ poly(amide acid) prepreg tape . that is, a prepreg tape from which the NMP solvent had not been removed. In the present process, one or more layer(s) of side-by-side boron fibers are pressed between dry prepreg tapes that have been prepared by the aforementioned gwet to dry h process. The multilayer tape is then heated to imidize the matrix material and remove most of the remaining solvent, and is pressed to consolidate the multiple layers into a dense tape. For tests, specimens of HYCARB tapes and laminated composite panels made from HYCARB tape were prepared as follows: HYCARB tapes were fabricated as described above. Each panel was made by laying down ten layers of tape, containing, variously, one, two, or three boron-fiber plies and the remainder carbon- fiber-only plies (see figure). Each panel was made by laying down ten layers of tape. Each panel was then cured by heating to a temperature of 225 C for 15 minutes, then pressing at 200 psi (A1.4 MPa) while heating to 371 C, holding at 371 C for 1 hour, then continuing to hold pressure during cooling. Control specimens that were otherwise identical except that they did not contain boron fibers also were prepared. In room-temperature flexural tests, the HYCARB specimens performed comparably to the control specimens; in room-temperature, open-hole compression tests, the HYCARB specimens performed slightly better, by amounts that increased with boron content.

Linear and Star Poly(ionic liquid) Assemblies: Surface Monolayers and Multilayers.

PubMed

Erwin, Andrew J; Xu, Weinan; He, Hongkun; Matyjaszewski, Krzysztof; Tsukruk, Vladimir V

2017-04-04

The surface morphology and organization of poly(ionic liquid)s (PILs), poly[1-(4-vinylbenzyl)-3-butylimidazolium bis(trifluoromethylsulfonyl)imide] are explored in conjunction with their molecular architecture, adsorption conditions, and postassembly treatments. The formation of stable PIL Langmuir and Langmuir-Blodgett (LB) monolayers at the air-water and air-solid interfaces is demonstrated. The hydrophobic bis(trifluoromethylsulfonyl)imide (Tf 2 N - ) is shown to be a critical agent governing the assembly morphology, as observed in the reversible condensation of LB monolayers into dense nanodroplets. The PIL is then incorporated as an unconventional polyelectrolyte component in the layer-by-layer (LbL) films of hydrophobic character. We demonstrate that the interplay of capillary forces, macromolecular mobility, and structural relaxation of the polymer chains influence the dewetting mechanisms in the PIL multilayers, thereby enabling access to a diverse set of highly textured, porous, and interconnected network morphologies for PIL LbL films that would otherwise be absent in conventional LbL films. Their compartmentalized internal structure is relevant to molecular separation membranes, ultrathin hydrophobic coatings, targeted cargo delivery, and highly conductive films.

Characterization of 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([Emim][Tf2N])∕TX-100∕cyclohexane ternary microemulsion: investigation of photoinduced electron transfer in this RTIL containing microemulsion.

PubMed

Sarkar, Souravi; Pramanik, Rajib; Ghatak, Chiranjib; Rao, Vishal Govind; Sarkar, Nilmoni

2011-02-21

In this study we have characterized a ionic liquid 1-ethyl-3-methylimidazolium bis(trifluoromethyl- sulfonyl)imide containing ternary nonaqueous microemulsion ([Emim][Tf(2)N]∕∕TX-100∕cyclo- hexane). The phase behavior and dynamic light scattering study show that the [Emim][Tf(2)N]∕TX-100∕cyclohexane three component system can form microemulsion with [Emim][Tf(2)N] as polar core at suitable condition. We have investigated photoinduced electron transfer (PET) using dimethyl aniline as electron donor and several Coumarin dyes as electron acceptor molecules at two different R values (R = [ionic liquid]∕[surfactant]) to observe how the dynamics of the PET rate is affected in this type of confined microenvironment compared to that of the PET dynamics in neat ionic liquid and other pure solvent media. The plot of observed k(q) values with the free energy change (ΔG(0)) for electron transfer reaction shows an apparent inversion in the observed rate as predicted by the Marcus theory.

Graphite fiber polyimide composites for spherical bearings to 340 C (650 F)

NASA Technical Reports Server (NTRS)

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

1972-01-01

Journal bearings with self-alining spherical elements of graphite-fiber-reinforced-polyimide composites were tested from 24 to 340 C (75 to 650 F) at unit loads up to 3.5 times 10 to the 7th power N/sq m (5000 psi). The journal oscillated in the cylindrical bore of the composite element + or - 15 deg at 1 hertz. Outer races and journals were metal hardened of Rockwell C-32 and finished to 10 to the minus 7th power m. A 45 wt. percent graphite-fiber composite gave low friction (0.08 to 0.13), low wear, and almost no plastic deformation under any of the test conditions. Composites with 15 and 25 wt. percent graphite fiber failed by plastic deformation at 315 C (600 F) and 3.5 times 10 to the 7th power N/sq m (5000 psi). A composite with 60 wt. percent graphite fiber failed by brittle fracture under the same conditions, but had very low friction coefficients (0.05 to 0.10) and may be a good bearing material at lighter loads.

Method of Forming a Composite Coating with Particle Materials that are Readily Dispersed in a Sprayable Polyimide Solution

NASA Technical Reports Server (NTRS)

Tran, Sang Q. (Inventor)

1998-01-01

A method for creating a composite form of coating from a sprayable solution of soluble polyimides and particle materials that are uniformly dispersed within the solution is described. The coating is formed by adding a soluble polyimide to a solvent, then stirring particle materials into the solution. The composite solution is sprayed onto a substrate and heated in an oven for a period of time in order to partially remove the solvent. The process may be repeated until the desired thickness or characteristic of the coating is obtained. The polyimide is then heated to at least 495 F, so that it is no longer soluble.

Surface modification of a polyimide gate insulator with an yttrium oxide interlayer for aqueous-solution-processed ZnO thin-film transistors.

PubMed

Jang, Kwang-Suk; Wee, Duyoung; Kim, Yun Ho; Kim, Jinsoo; Ahn, Taek; Ka, Jae-Won; Yi, Mi Hye

2013-06-11

We report a simple approach to modify the surface of a polyimide gate insulator with an yttrium oxide interlayer for aqueous-solution-processed ZnO thin-film transistors. It is expected that the yttrium oxide interlayer will provide a surface that is more chemically compatible with the ZnO semiconductor than is bare polyimde. The field-effect mobility and the on/off current ratio of the ZnO TFT with the YOx/polyimide gate insulator were 0.456 cm(2)/V·s and 2.12 × 10(6), respectively, whereas the ZnO TFT with the polyimide gate insulator was inactive.

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.

The electrical conductivities of polyimide and polyimide/Li triflate composites: An a.c. impedance study

NASA Astrophysics Data System (ADS)

Aziz, Nor Diyana Abdul; Kamarulzaman, Norlida; Subban, Ri Hanum Yahaya; Hamzah, Ahmad Sazali; Ahmed, Azni Zain; Osman, Zurina; Rusdi, Roshidah; Kamarudin, Norashikin; Mohalid, Norhanim; Romli, Ahmad Zafir; Shaameri, Zurina

2017-09-01

Polymer electrolytes have been an essential area of research for many decades. One of the reasons was the need to find new electrolyte materials suitable for device applications like solid-state batteries, supercapacitors, fuel cells, etc. with enhanced characteristics. For more than 40 years, polyimide has been known as a super-engineering plastic due to its excellent thermal stability (Tg > 250 °C) and mechanical properties. Therefore, in an effort to develop new polymer electrolytes, polyimide as a polymer matrix was chosen. Composite films of the polymer doped with lithium salt, LiCF3SO3 was prepared. These PI based polymer electrolyte films were investigated by the alternating current (a.c.) impedance spectroscopy method in the temperature range from 300 K to 373 K. It was observed that conductivity increased with the increase of temperature and amount of doping salt. Alternatively, the activation energy (Ea) of the composite films decreased with the increase of the doping salt, LiCF3SO3.

Study on Thermal Conductivities of Aromatic Polyimide Aerogels.

PubMed

Feng, Junzong; Wang, Xin; Jiang, Yonggang; Du, Dongxuan; Feng, Jian

2016-05-25

Polyimide aerogels for low density thermal insulation materials were produced by 4,4'-diaminodiphenyl ether and 3,3',4,4'-biphenyltetracarboxylic dianhydride, cross-linked with 1,3,5-triaminophenoxybenzene. The densities of obtained polyimide aerogels are between 0.081 and 0.141 g cm(-3), and the specific surface areas are between 288 and 322 m(2) g(-1). The thermal conductivities were measured by a Hot Disk thermal constant analyzer. The value of the measured thermal conductivity under carbon dioxide atmosphere is lower than that under nitrogen atmosphere. Under pressure of 5 Pa at -130 °C, the thermal conductivity is the lowest, which is 8.42 mW (m K)(-1). The polyimide aerogels have lower conductivity [30.80 mW (m K)(-1)], compared to the value for other organic foams (polyurethane foam, phenolic foam, and polystyrene foam) with similar apparent densities under ambient pressure at 25 °C. The results indicate that polyimide aerogel is an ideal insulation material for aerospace and other applications.

Flexible polyimides through one-pot synthesis as water-soluble binders for silicon anodes in lithium ion batteries

NASA Astrophysics Data System (ADS)

Yao, Dahua; Yang, Yu; Deng, Yonghong; Wang, Chaoyang

2018-03-01

A series of polyimides, which contain polyethylene glycol (PEG) segments with different molecular weight in the polymer chains, are synthesized through a facile one-pot method and characterized by Fourier transform infrared spectroscopy and hydrogen nuclear magnetic resonance spectroscopy. The main part of polyimides is originated from trimellitic anhydride chloride (TMAC) and 4,4‧-methylenedianiline, onto which PEG segments are introduced through an esterification reaction with TMAC. These obtained polyimides, which acquire excellent water solubility after being neutralized by triethylamine, are applied as water-soluble binders to silicon negative electrodes for lithium ion batteries, and significantly improve the electrochemical performance of silicon anodes. Specially, the PI-200 (polyimide copolymerized with PEG-200) based silicon electrode exhibits a high initial discharge capacity of 2989.7 mAh g-1 and remains about 2235.5 mAh g-1 after 200 cycles at the current density of 0.1 C (420 mA g-1).

Process for preparing essentially colorless polyimide film containing phenoxy-linked diamines

NASA Technical Reports Server (NTRS)

Stclair, A. K.; Stclair, T. L.

1986-01-01

A polyimide film that is approximately 90% transparent at 500 nm, useful for thermal protective coatings and solar cells, and the processes for preparing the same by thermal and chemical conversion are disclosed. An essential feature for achieving maximum optical transparency films requires utilizing recrystallized and/or sublimated specific aromatic diamines and dianhydride monomers and introducing phenoxy or thiophenyl separator groups and isomeric m,m' or o,p'-oriented diamines into the polymer molecular structure. The incorporation of these groups in the polymer structure serves to separate the chromaphoric centers and reduce the formation of inter-chain and intra-chain charge transfer complexes which normally cause absorptions in the UV-visible range. The films may be obtained by hand, brushing, casting, or spraying a layer of polyamic acid solutions onto a surface and thermally converting the applied layer to the polyimide, or the polyamic acid solution can be chemically converted to the polyimide, subsequentially dissolved in an organic solvent, and applied as a polyimide film layer with the solvent therein thermally removed.

Prediction of Mechanical Properties of Polymers With Various Force Fields

NASA Technical Reports Server (NTRS)

Odegard, Gregory M.; Clancy, Thomas C.; Gates, Thomas S.

2005-01-01

The effect of force field type on the predicted elastic properties of a polyimide is examined using a multiscale modeling technique. Molecular Dynamics simulations are used to predict the atomic structure and elastic properties of the polymer by subjecting a representative volume element of the material to bulk and shear finite deformations. The elastic properties of the polyimide are determined using three force fields: AMBER, OPLS-AA, and MM3. The predicted values of Young s modulus and shear modulus of the polyimide are compared with experimental values. The results indicate that the mechanical properties of the polyimide predicted with the OPLS-AA force field most closely matched those from experiment. The results also indicate that while the complexity of the force field does not have a significant effect on the accuracy of predicted properties, small differences in the force constants and the functional form of individual terms in the force fields determine the accuracy of the force field in predicting the elastic properties of the polyimide.

Microstructural Characterization of Semi-Interpenetrating Polymer Networks by Positron Lifetime Spectroscopy

NASA Technical Reports Server (NTRS)

Singh, Jag J.; Pater, Ruth H.; Eftekhari, Abe

1996-01-01

Thermoset and thermoplastic polyimides have complementary physical and mechanical properties. Whereas thermoset polyimides are brittle and generally easier to process, thermoplastic polyimides are tough but harder to process. A combination of these two types of polyimides may help produce polymers more suitable for aerospace applications. Semi-Interpenetrating Polymer Networks (S-IPN) of thermoset LaRC(TM)-RP46 and thermoplastic LaRC(TM)-IA polyimides were prepared in weight percent ratios ranging from 100:0 to 0:100. Positron lifetime measurements were made in these samples to correlate their free volume features with physical and mechanical properties. As expected, positronium atoms are not formed in these samples. The second lifetime component has been used to infer the positron trap dimensions. The 'free volume' goes through a minimum at a ratio of about 50:50, and this suggests that S-IPN samples are not merely solid solutions of the two polymers. These data and related structural properties of the S-IPN samples are discussed.

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.

Microfabricated Multianalyte Sensor Arrays for Metabolic Monitoring

DTIC Science & Technology

2006-09-01

aqueous in vivo-like surrounding15-18 to entrap both the redox polymer and glucose oxidase on polyimide sheets. We have used biocompatible PEG-DA hydrogel...arrays were fabricated on gold electrodes on flexible polyimide sheets by cross-linking glucose oxidase and redox polymer using UV-initiated free...cyclic voltammetry. We have fabricated an array of glucose sensors on flexible polyimide sheets that exhibit the desired linear response in the

Polyimides Containing Silver Trifluoroacetylacetonate

NASA Technical Reports Server (NTRS)

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

1994-01-01

Mechanically strong, flexible, thermally stable, electrically conductive films and coatings suitable for use in electronics industry made by incorporating silver trifluoroacetylacetonate into linear aromatic condensation polyimides. In experimental films, most successful combinations of flexibility and conductivity obtained by use of 1:1, 1:1.74, and 1:2 mole ratios of silver trifluoroacetylacetonate per polyimide repeat unit. Other concentrations of silver trifluoroacetylacetonate used with different heat-treatment schedules to obtain conductive silver-impregnated films.

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.

Electro-optical and physic-mechanical properties of colored alicyclic polyimide

NASA Astrophysics Data System (ADS)

Kravtsova, V.; Umerzakova, M.; Korobova, N.; Timoshenkov, S.; Timoshenkov, V.; Orlov, S.; Iskakov, R.; Prikhodko, O.

2016-09-01

Main optical, thermal and mechanical properties of new compositions based on alicyclic polyimide and active bright red 6C synthetic dye have been studied. It was shown that the transmission ratio of the new material in the region of 400-900 nm and 2.0 wt.% dye concentration was around 60-70%. Thermal, mechanical and electrical properties of new colored compositions were comparable with the properties of original polyimide.

2,2-Bis[(2-halo-4-aminophenoxy)phenyl]-hexafluoropropane

NASA Technical Reports Server (NTRS)

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

1985-01-01

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.

Polished polymide substrate

DOEpatents

Farah, John; Sudarshanam, Venkatapuram S.

2003-05-13

Polymer substrates, in particular polyimide substrates, and polymer laminates for optical applications are described. Polyimide substrates are polished on one or both sides depending on their thickness, and single-layer or multi-layer waveguide structures are deposited on the polished polyimide substrates. Optical waveguide devices are machined by laser ablation using a combination of IR and UV lasers. A waveguide-fiber coupler with a laser-machined groove for retaining the fiber is also disclosed.

Polarization and Piezoelectric Properties of a Nitrile Substituted Polyimide

NASA Technical Reports Server (NTRS)

Simpson, Joycelyn; Ounaies, Zoubeida; Fay, Catharine

1997-01-01

This research focuses on the synthesis and characterization of a piezoelectric (beta-CN)- APB/ODPA polyimide. The remanent polarization and piezoelectric d(sub 31) and g(sub 33) coefficients are reported to assess the effect of synthesis variations. Each of the materials exhibits a level of piezoelectricity which increases with temperature. The remanent polarization is retained at temperatures close to the glass transition temperature of the polyimide.

Atomic Oxygen Effects on POSS Polyimides

DTIC Science & Technology

2011-07-25

resistance to UV damage, and excellent thermal properties.1 Despite the desirable properties of Kapton, this polyimide and all organic polymeric materials...stability, insulation properties, IR transparency, low solar absorptance, resistance to UV damage, and excellent thermal properties.1 Despite the...8 × 1021 atoms cm-2. Free standing films of MC-POSS polyimide were sewn to a Kapton blanket and exposed to a sweeping ram in LEO on MISSE-5

Gas Permeation Properties of Soluble Aromatic Polyimides Based on 4-Fluoro-4,4'-Diaminotriphenylmethane

PubMed Central

Guzmán-Lucero, Diego; Froylán Palomeque-Santiago, Jorge; Camacho-Zúñiga, Claudia; Ruiz-Treviño, Francisco Alberto; Guzmán, Javier; Galicia-Aguilar, Alberto; Aguilar-Lugo, Carla

2015-01-01

A series of new organic polyimides were synthesized from 4-fluoro-4'4"-diaminotriphenylmethane and four different aromatic dianhydrides through a one-step, high-temperature, direct polycondensation in m-cresol at 180–200 °C, resulting in the formation of high-molecular-weight polyimides (inherent viscosities ~ 1.0–1.3 dL/g). All the resulting polyimides exhibited good thermal stability with initial decomposition temperatures above 434 °C, glass-transition temperatures between 285 and 316 °C, and good solubility in polar aprotic solvents. Wide-angle X-ray scattering data indicated that the polyimides were amorphous. Dense membranes were prepared by solution casting and solvent evaporation to evaluate their gas transport properties (permeability, diffusivity, and solubility coefficients) toward pure hydrogen, helium, oxygen, nitrogen, methane, and carbon dioxide gases. In general, the gas permeability was increased as both the fractional free volume and d-spacing were also increased. A good combination of permeability and selectivity was promoted efficiently by the bulky hexafluoroisopropylidene and 4-fluoro-phenyl groups introduced into the polyimides. The results indicate that the gas transport properties of these films depend on both the structure of the anhydride moiety, which controls the intrinsic intramolecular rigidity, and the 4-fluoro-phenyl pendant group, which disrupts the intermolecular packing. PMID:28788041

Gas Permeation Properties of Soluble Aromatic Polyimides Based on 4-Fluoro-4,4'-Diaminotriphenylmethane.

PubMed

Guzmán-Lucero, Diego; Palomeque-Santiago, Jorge Froylán; Camacho-Zúñiga, Claudia; Ruiz-Treviño, Francisco Alberto; Guzmán, Javier; Galicia-Aguilar, Alberto; Aguilar-Lugo, Carla

2015-04-21

A series of new organic polyimides were synthesized from 4-fluoro-4'4"-diaminotriphenylmethane and four different aromatic dianhydrides through a one-step, high-temperature, direct polycondensation in m-cresol at 180-200 °C, resulting in the formation of high-molecular-weight polyimides (inherent viscosities ~ 1.0-1.3 dL/g). All the resulting polyimides exhibited good thermal stability with initial decomposition temperatures above 434 °C, glass-transition temperatures between 285 and 316 °C, and good solubility in polar aprotic solvents. Wide-angle X-ray scattering data indicated that the polyimides were amorphous. Dense membranes were prepared by solution casting and solvent evaporation to evaluate their gas transport properties (permeability, diffusivity, and solubility coefficients) toward pure hydrogen, helium, oxygen, nitrogen, methane, and carbon dioxide gases. In general, the gas permeability was increased as both the fractional free volume and d-spacing were also increased. A good combination of permeability and selectivity was promoted efficiently by the bulky hexafluoroisopropylidene and 4-fluoro-phenyl groups introduced into the polyimides. The results indicate that the gas transport properties of these films depend on both the structure of the anhydride moiety, which controls the intrinsic intramolecular rigidity, and the 4-fluoro-phenyl pendant group, which disrupts the intermolecular packing.

Polyimide as a versatile enabling material for microsystems fabrication: surface micromachining and electrodeposited nanowires integration

NASA Astrophysics Data System (ADS)

Walewyns, Thomas; Reckinger, Nicolas; Ryelandt, Sophie; Pardoen, Thomas; Raskin, Jean-Pierre; Francis, Laurent A.

2013-09-01

The interest of using polyimide as a sacrificial and anchoring layer is demonstrated for post-processing surface micromachining and for the incorporation of metallic nanowires into microsystems. In addition to properties like a high planarization factor, a good resistance to most non-oxidizing acids and bases, and CMOS compatibility, polyimide can also be used as a mold for nanostructures after ion track-etching. Moreover, specific polyimide grades, such as PI-2611 from HD Microsystems™, involve a thermal expansion coefficient similar to silicon and low internal stress. The process developed in this study permits higher gaps compared to the state-of-the-art, limits stiction problems with the substrate and is adapted to various top-layer materials. Most metals, semiconductors or ceramics will not be affected by the oxygen plasma required for polyimide etching. Released structures with vertical gaps from one to several tens of μm have been obtained, possibly using multiple layers of polyimide. Furthermore, patterned freestanding nanowires have been synthesized with diameters from 20 to 60 nm and up to 3 μm in length. These results have been applied to the fabrication of two specific devices: a generic nanomechanical testing lab-on-chip platform and a miniaturized ionization sensor.

Thermoresponsive light scattering device utilizing surface behavior effects between polyimide and an ionic liquid-water mixture exhibiting lower critical solution temperature (LCST)-type phase separation

NASA Astrophysics Data System (ADS)

Goda, Kazuya; Takatoh, Kohki; Funasako, Yusuke; Inokuchi, Makoto

2018-06-01

We proposed a thermoresponsive light scattering device that utilizes the surface behavior between polyimide and an ionic liquid-water mixture exhibiting lower critical solution temperature (LCST)-type phase separation. The LCST behavior for an ionic liquid device utilizing the polyimide with and without alkyl side chains was investigated. In the here-reported ionic liquid device that utilized the polyimide with alkyl side chains, [nBu4P][CF3COO] droplets were generated by phase separation—they were predominantly formed at the alkyl surface by a surface pinning effect. A stable transmittance in the opaque state could be obtained with this device. In contrast, an ionic liquid device using polyimide without alkyl side chains deteriorated transmittance in the opaque state because there was no surface pinning effect. Additionally, the viewing angle, contrast ratio, and heat cycle testing of this ionic liquid device with polyimide with alkyl side chains were also investigated. The results indicated that no parallax was obtained and that the ionic liquid device has a stable transmittance (verified by heat cycle testing). This unique device is expected to find use in the smart window applications that are activated by temperature changes.

Effect of integrated infectious disease training and on-site support on the management of childhood illnesses in Uganda: a cluster randomized trial.

PubMed

Imani, Peace; Jakech, Brian; Kirunda, Ibrahim; Mbonye, Martin K; Naikoba, Sarah; Weaver, Marcia R

2015-08-28

The Integrated Infectious Disease Capacity-Building Evaluation (IDCAP) was designed to test the effects of two interventions, Integrated Management of Infectious Disease (IMID) training and on-site support (OSS), on clinical practice of mid-level practitioners. This article reports the effects of these interventions on clinical practice in management of common childhood illnesses. Two trainees from each of 36 health facilities participated in the IMID training. IMID was a three-week core course, two one-week boost courses, and distance learning over nine months. Eighteen of the 36 health facilities were then randomly assigned to arm A, and participated in OSS, while the other 18 health facilities assigned to arm B did not. Clinical faculty assessed trainee practice on clinical practice of six sets of tasks: patient history, physical examination, laboratory tests, diagnosis, treatment, and patient/caregiver education. The effects of IMID were measured by the post/pre adjusted relative risk (aRR) of appropriate practice in arm B. The incremental effects of OSS were measured by the adjusted ratio of relative risks (aRRR) in arm A compared to arm B. All hypotheses were tested at a 5% level of significance. Patient samples were comparable across arms at baseline and endline. The majority of children were aged under five years; 84% at baseline and 97% at endline. The effects of IMID on patient history (aRR = 1.12; 95% CI = 1.04-1.21) and physical examination (aRR = 1.40; 95% CI = 1.16-1.68) tasks were statistically significant. OSS was associated with incremental improvement in patient history (aRRR = 1.18; 95% CI = 1.06-1.31), and physical examination (aRRR = 1.27; 95% CI = 1.02-1.59) tasks. Improvements in laboratory testing, diagnosis, treatment, and patient/caregiver education were not statistically significant. IMID training was associated with improved patient history taking and physical examination, and OSS further improved these clinical practices. On-site training and continuous quality improvement activities support transfer of learning to practice among mid-level practitioners.

Surface Polarity and Self-Structured Nanogrooves Collaboratively Oriented Molecular Packing for High Crystallinity toward Efficient Charge Transport.

PubMed

Ji, Deyang; Xu, Xiaomin; Jiang, Longfeng; Amirjalayer, Saeed; Jiang, Lang; Zhen, Yonggang; Zou, Ye; Yao, Yifan; Dong, Huanli; Yu, Junsheng; Fuchs, Harald; Hu, Wenping

2017-02-22

Efficient charge transport in organic semiconductors is essential for construction of high performance optoelectronic devices. Herein, for the first time, we demonstrate that poly(amic acid) (PAA), a facilely deposited and annealing-free dielectric layer, can tailor the growth of organic semiconductor films with large area and high crystallinity toward efficient charge transport and high mobility in their thin film transistors. Pentacene is used as a model system to demonstrate the concept with mobility up to 30.6 cm 2 V -1 s -1 , comparable to its high quality single crystal devices. The structure of PAA has corrugations with OH groups pointing out of the surface, and the presence of an amide bond further allows adjacent polymer strands to interact via hydrogen bonding, leading to a self-rippled surface perpendicular to the corrugation. On the other hand, the strong polar groups (-COOH/-CONH) of PAA could provide repulsive forces between PAA and pentacene, which results in the vertical orientation of pentacene on the dielectric surface. Indeed, in comparison with its imidized counterpart polyimide (PI), PAA dielectric significantly enhances the film crystallinity, drastically increases the domain size, and decreases the interface trap density, giving rise to superior device performance with high mobility. This concept can be extended to more organic semiconducting systems, e.g., 2,6-diphenylanthracene (DPA), tetracene, copper phthalocyanine (CuPc), and copper hexadecafluorophthalocyanine (F 16 CuPc), demonstrating the general applicability. The results show the importance of combining surface nanogrooves with the strong polarity in orienting the molecular arrangement for high crystallinity toward efficient charge transport in organic semiconductors.

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.

Anodic Behavior of the Aluminum Current Collector in Imide-Based Electrolytes: Influence of Solvent, Operating Temperature, and Native Oxide-Layer Thickness.

PubMed

Meister, Paul; Qi, Xin; Kloepsch, Richard; Krämer, Elisabeth; Streipert, Benjamin; Winter, Martin; Placke, Tobias

2017-02-22

The inability of imide salts to form a sufficiently effective passivation layer on aluminum current collectors is one of the main obstacles that limit their broad application in electrochemical energy-storage systems. However, under certain circumstances, the use of electrolytes with imide electrolyte salts in combination with the aluminum current collector is possible. In this contribution, the stability of the aluminum current collector in electrolytes containing either lithium bis(trifluoromethanesulfonyl) imide (LiTFSI) or lithium fluorosulfonyl-(trifluoromethanesulfonyl) imide (LiFTFSI) as conductive salt was investigated by electrochemical techniques, that is, cyclic voltammetry (CV) and chronocoulometry (CC) in either room-temperature ionic liquids or in ethyl methyl sulfone. In particular, the influence of the solvent, operating temperature, and thickness of the native oxide layer of aluminum on the pit formation at the aluminum current collector surface was studied by means of scanning electron microscopy. In general, a more pronounced aluminum dissolution and pit formation was found at elevated temperatures as well as in solvents with a high dielectric constant. An enhanced thickness of the native aluminum oxide layer increases the oxidative stability versus dissolution. Furthermore, we found a different reaction rate depending on dwell time at the upper cut-off potential for aluminum dissolution in TFSI- and FTFSI-based electrolytes during the CC measurements; the use of LiFTFSI facilitated the dissolution of aluminum compared to LiTFSI. Overall, the mechanism of anodic aluminum dissolution is based on: i) the attack of the Al 2 O 3 surface by acidic species and ii) the dissolution of bare aluminum into the electrolyte, which, in turn, is influenced by the electrolyte's dielectric constant. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Pomalidomide desensitization in a patient hypersensitive to immunomodulating agents

PubMed Central

Seki, J.T.; Sakurai, N.; Lam, W.; Reece, D.E.

2017-01-01

Despite progressive treatments with tandem stem-cell transplantation, patients with incurable myeloma eventually succumb to relapsed or refractory disease if left untreated. Promising agents such as proteasome inhibitors and immunomodulating imide drugs (imids), including the newer-generation agent pomalidomide, in combination with lower-dose dexamethasone, have been shown to be effective and to significantly improve and prolong survival in pretreated patients. Although the incidence of pomalidomide hypersensitivity reaction (hsr) in this class of drugs is not as well known, we have documented cutaneous toxicity (grade 3 by the Common Terminology Criteria for Adverse Events, version 4) in 2 separate cases (not yet published). Because the imids are chemically, structurally, and pharmacologically similar, it is not unreasonable to consider possible cross-reactivity in pomalidomide recipients who developed hsr when receiving previous lines of imids. As a patient’s advocate, it is only prudent to provide a responsible, and yet practical, means to better address cross-sensitivity for patients. Intervention with the use of a rapid desensitization program (rdp) as a preventive measure should be introduced before initiating pomalidomide. Such a proactive measure for the patient’s safety will ensure a smooth transition into pomalidomide treatment. A hsr can be either related or non-related to immunoglobulin E. As imids become an essential treatment backbone for myeloma and other plasma-cell diseases, an increasing number of patients could experience skin and other life-threatening toxicities, resulting in unnecessary discontinuation of these life-prolonging agents. An extemporaneously prepared pomalidomide suspension developed at our centre enables patients to undergo rdp safely. Patients enjoy a good quality of life and clinical response after the rdp procedure. PMID:28874903

Cost-effectiveness of an influenza vaccination program offering intramuscular and intradermal vaccines versus intramuscular vaccine alone for elderly.

PubMed

Leung, Man-Kit; You, Joyce H S

2016-05-11

Intradermal (ID) injection is an alternative route for influenza vaccine administration in elderly with potential improvement of vaccine coverage. This study aimed to investigate the cost-effectiveness of an influenza vaccination program offering ID vaccine to elderly who had declined intramuscular (IM) vaccine from the perspective of Hong Kong public healthcare provider. A decision analytic model was used to simulate outcomes of two programs: IM vaccine alone (IM program), and IM or ID vaccine (IM/ID program) in a hypothetic cohort of elderly aged 65 years. Outcome measures included influenza-related direct medical cost, infection rate, mortality rate, quality-adjusted life years (QALYs) loss, and incremental cost per QALY saved (ICER). Model inputs were derived from literature. Sensitivity analyses evaluated the impact of uncertainty of model variables. In base-case analysis, the IM/ID program was more costly (USD52.82 versus USD47.59 per individual to whom vaccine was offered) with lower influenza infection rate (8.71% versus 9.65%), mortality rate (0.021% versus 0.024%) and QALYs loss (0.00336 versus 0.00372) than the IM program. ICER of IM/ID program was USD14,528 per QALY saved. One-way sensitivity analysis found ICER of IM/ID program to exceed willingness-to-pay threshold (USD39,933) when probability of influenza infection in unvaccinated elderly decreased from 10.6% to 5.4%. In 10,000 Monte Carlo simulations of elderly populations of Hong Kong, the IM/ID program was the preferred option in 94.7% of time. An influenza vaccination program offering ID vaccine to elderly who had declined IM vaccine appears to be a highly cost-effective option. Copyright © 2016 Elsevier Ltd. All rights reserved.

Glutamic Acid Selective Chemical Cleavage of Peptide Bonds.

PubMed

Nalbone, Joseph M; Lahankar, Neelam; Buissereth, Lyssa; Raj, Monika

2016-03-04

Site-specific hydrolysis of peptide bonds at glutamic acid under neutral aqueous conditions is reported. The method relies on the activation of the backbone amide chain at glutamic acid by the formation of a pyroglutamyl (pGlu) imide moiety. This activation increases the susceptibility of a peptide bond toward hydrolysis. The method is highly specific and demonstrates broad substrate scope including cleavage of various bioactive peptides with unnatural amino acid residues, which are unsuitable substrates for enzymatic hydrolysis.

Lithium insertion in graphite from ternary ionic liquid-lithium salt electrolytes: II. Evaluation of specific capacity and cycling efficiency and stability at room temperature

NASA Astrophysics Data System (ADS)

Lux, Simon F.; Schmuck, Martin; Appetecchi, Giovanni B.; Passerini, Stefano; Winter, Martin; Balducci, Andrea

In this paper we report the results about the use of ternary room temperature ionic liquid-lithium salt mixtures as electrolytes for lithium-ion battery systems. Mixtures of N-methyl- N-propyl pyrrolidinium bis(fluorosulfonyl) imide, PYR 13FSI, and N-butyl- N-methylpyrrolidinium bis(trifluoromethansulfonyl) imide, PYR 14TFSI, with lithium hexafluorophosphate, LiPF 6 and lithium bis(trifluoromethansulfonyl) imide, LiTFSI, containing 5 wt.% of vinylene carbonate (VC) as additive, have been used in combination with a commercial graphite, KS6 TIMCAL. The performance of the graphite electrodes has been considered in term of specific capacity, cycling efficiency and cycling stability. The results clearly show the advantage of the use of ternary mixtures on the performance of the graphite electrode.

New Poly(amide-imide)/Nanocomposites Reinforced Silicate Nanoparticles Based on N-pyromellitimido-L-phenyl Alanine Containing Ether Moieties

NASA Astrophysics Data System (ADS)

Faghihi, Khalil; Shabanian, Meisam; Dadfar, Ehsan

2012-02-01

A series of Poly(amide-imide)/montmorillonite nanocomposites containing N-pyromellitimido-L-phenyl alanine moiety in the main chain were synthesized by a convenient solution intercalation technique. Poly(amide-imide) (PAI) 5 as a source of polymer matrix was synthesized by the direct polycondensation reaction of N-pyromellitimido-L-phenyl alanine 3 with 4,4'-diamino diphenyl ether 4 in the presence of triphenyl phosphite (TPP), CaCl2, pyridine and N-methyl-2-pyrrolidone (NMP). The resulting nanocomposite films were characterized by Fourier transform infrared spectra (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). The results showed that organo-modified clay was dispersed homogeneously in PAI matrix. TGA indicated an enhancement of thermal stability of new nanocomposites compared with the pure polymer.

Thermal and Optical Properties of New Poly(amide-imide)/Nanocomposite Reinforced by Layer Silicate Containing Diphenyl Ether Moieties

NASA Astrophysics Data System (ADS)

Faghihi, Khalil; Faramarzi, Ellahe; Shabanian, Meisam

2011-04-01

New poly(amide-imide)-montmorillonite reinforced nanocomposites containing Bis(4-N-trimellitylimido) diphenyl ether moiety in the main chain were synthesized by a convenient solution intercalation technique. Poly(amide-imide) (PAI) 4 was synthesized by the direct polycondensation reaction of Bis(4-N-trimellitylimido) diphenyl ether 3 with 4,4'-diamino diphenyl ether 2 in the presence of triphenyl phosphite (TPP), CaCl2, pyridine and N-methyl-2-pyrrolidone (NMP). Morphology and structure of the resulting PAI-nanocomposite films 4a and 4b with 10 and 20 mass% silicate particles respectively, were characterized by FT-IR spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The properties of nanocomposites films were investigated by using Uv-vis spectroscopy, thermogravimetric analysis (TGA) and water uptake measurements.

Micro-Fabricated Perforated Polymer Devices for Long-Term Drug Delivery

DTIC Science & Technology

2011-02-24

conventional manufacturing methods. We have used a biocompatible polymer ( polyimide ) to serve as a reservoir and photolithographically produced microholes for...RIE with ICP source was used to etch holes on polyimide surface. Biocompatible materials Ti, SiO2 and SiNx were studied as mask materials. Ti film...used to fabricate micro holes on the surface of polyimide tubes. Several materials have been used to form the etching mask, including titanium film

The characteristics of polyimide photoalignment layer with chalcone derivatives produced by linear polarized UV light

NASA Astrophysics Data System (ADS)

Jung, Kyoung Hoon; Hyun, Soon-Young; Song, Dong-Mee; Shin, Dong-Myung

2003-01-01

The photoalignment of liquid crystal (LC) molecules located onto polyimide films with chalcone derivatives using linearly polarized UV (LPUV) light is investigated. The LPUV light irradiation generated dimerization products of the chalcones followed by isomerization of the chalcone derivatives. The alignment directions of LC molecules were either homeotropic or planar with respect to plane of polyimide film, depending upon the alkyl chain length attached on the chalcones.

The association of fatigue, pain, depression and anxiety with work and activity impairment in immune mediated inflammatory diseases.

PubMed

Enns, Murray W; Bernstein, Charles N; Kroeker, Kristine; Graff, Lesley; Walker, John R; Lix, Lisa M; Hitchon, Carol A; El-Gabalawy, Renée; Fisk, John D; Marrie, Ruth Ann

2018-01-01

Impairment in work function is a frequent outcome in patients with chronic conditions such as immune-mediated inflammatory diseases (IMID), depression and anxiety disorders. The personal and economic costs of work impairment in these disorders are immense. Symptoms of pain, fatigue, depression and anxiety are potentially remediable forms of distress that may contribute to work impairment in chronic health conditions such as IMID. The present study evaluated the association between pain [Medical Outcomes Study Pain Effects Scale], fatigue [Daily Fatigue Impact Scale], depression and anxiety [Hospital Anxiety and Depression Scale] and work impairment [Work Productivity and Activity Impairment Scale] in four patient populations: multiple sclerosis (n = 255), inflammatory bowel disease (n = 248, rheumatoid arthritis (n = 154) and a depression and anxiety group (n = 307), using quantile regression, controlling for the effects of sociodemographic factors, physical disability, and cognitive deficits. Each of pain, depression symptoms, anxiety symptoms, and fatigue individually showed significant associations with work absenteeism, presenteeism, and general activity impairment (quantile regression standardized estimates ranging from 0.3 to 1.0). When the distress variables were entered concurrently into the regression models, fatigue was a significant predictor of work and activity impairment in all models (quantile regression standardized estimates ranging from 0.2 to 0.5). These findings have important clinical implications for understanding the determinants of work impairment and for improving work-related outcomes in chronic disease.

Polyimide Cellulose Nanocrystal Composite Aerogels

NASA Technical Reports Server (NTRS)

Nguyen, Baochau N.; Meador, Mary Ann; Rowan, Stuart; Cudjoe, Elvis; Sandberg, Anna

2014-01-01

Polyimide (PI) aerogels are highly porous solids having low density, high porosity and low thermal conductivity with good mechanical properties. They are ideal for various applications including use in antenna and insulation such as inflatable decelerators used in entry, decent and landing operations. Recently, attention has been focused on stimuli responsive materials such as cellulose nano crystals (CNCs). CNCs are environmentally friendly, bio-renewable, commonly found in plants and the dermis of sea tunicates, and potentially low cost. This study is to examine the effects of CNC on the polyimide aerogels. The CNC used in this project are extracted from mantle of a sea creature called tunicates. A series of polyimide cellulose nanocrystal composite aerogels has been fabricated having 0-13 wt of CNC. Results will be discussed.

Development of new addition-type composite resins

NASA Technical Reports Server (NTRS)

Kray, R. J.

1981-01-01

The most promising of a number of new addition type polyimides and polyaromatic melamine (NCNS) resins for use in high performance composite materials. Three different cure temperature ranges were of interest: 530-560 K (500-550 F), 475-530 K (400-500 F), and 450 K (350 F). Examined were a wide variety of polyimide precursors terminated with 5 norbornene groups and addition polymerized at 560 K similar to PMR-15 and LARC-160 polyimides. In addition, a number of lower curing cinnamal end capped polyimides and a bismaleimide were investigated but were not found promising. A group of NCNS resins were investigated and some were found to be superior to current epoxy resins in moisture resistance, oxidative aging and flame and smoke properties.

A High T(sub g) PMR Polyimide Composites (DMBZ-15)

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.; Bowles, Kenneth J.; Papadopoulos, Demitrios S.; Hardy-Green, DeNise; Mccorkle, Linda

2000-01-01

A high T(sub g) thermosetting PMR-type polyimide, designated as DMBZ-15, was developed by replacing methylene dianline (MDA) in PMR-15 with 2,2'-dimethylbenzidine. Polyimide/carbon fiber (T650-35) composites were fabricated from a formulation of 3,3', 4,4'-benzophenonetetracarboxylic acid dimethyl ester (BTDE) and 2,2'-dimethylbenzidine (DMBZ), along with nadic ester (NE) as the endcap. DMBZ-15 displays a higher glass transition temperature (T(sub g) = 414 C) than PMR-15 (T(sub g) = 345 C), and thus retains better mechanical properties for brief exposure above 400 C. The physical properties and longterm thermo-oxidative stability of the DMBZ-15 polyimide/carbon fiber composites are also compared to that of PMR-15.

Fresnel Concentrators for Space Solar Power and Solar Thermal Propulsion

NASA Technical Reports Server (NTRS)

Bradford, Rodney; Parks, Robert W.; Craig, Harry B. (Technical Monitor)

2001-01-01

Large deployable Fresnel concentrators are applicable to solar thermal propulsion and multiple space solar power generation concepts. These concentrators can be used with thermophotovoltaic, solar thermionic, and solar dynamic conversion systems. Thin polyimide Fresnel lenses and reflectors can provide tailored flux distribution and concentration ratios matched to receiver requirements. Thin, preformed polyimide film structure components assembled into support structures for Fresnel concentrators provide the capability to produce large inflation-deployed concentrator assemblies. The polyimide film is resistant to the space environment and allows large lightweight assemblies to be fabricated that can be compactly stowed for launch. This work addressed design and fabrication of lightweight polyimide film Fresnel concentrators, alternate materials evaluation, and data management functions for space solar power concepts, architectures, and supporting technology development.

Novel polyimide compositions based on 4,4': Isophthaloyldiphthalic anaydride (IDPA)

NASA Technical Reports Server (NTRS)

Pratt, J. Richard (Inventor); Saintclair, Terry L. (Inventor)

1989-01-01

A series of twelve high temperature, high performance polyimide compositions based on 4,4'-isophthaloyl diphthalic anhydride (IDPA) was prepared and characterized. Tough, film-forming, organic solvent-insoluble polyimides were obtained. Three materials were semicrystalline. Several gave excellent long-term thermooxidative stability by isothermal thermogravimetric analysis (ITGA) at 300 C and 350 C in air when compared to Kapton H film (duPont). One extensively studied material displayed different levels of semicrystallinity over a wide range of final cure time/temperatures. The polyimide from IDPA and 1,3-bis (4-aminophenoxy 4'-benzoyl) benzene exhibited multiple crystallization and melting behavior, implying the existence of two kinetic and two thermodynamic crystallization and melting transitions by differential scanning calorimetry (DSC).

Imide/arylene ether copolymers

NASA Technical Reports Server (NTRS)

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

1992-01-01

Imide/arylene ether block copolymers are prepared by reacting anhydride terminated poly(amic acids) with amine terminated poly(arylene ethers) in polar aprotic solvents and by chemically or thermally cyclodehydrating the resulting intermediate poly(amic acids). The resulting block copolymers have one glass transition temperature or two, depending upon the particular structure and/or the compatibility of the block units. Most of these block copolymers form tough, solvent resistant films with high tensile properties.

Molecular structure of imide solutions. Part I. Propionimide in non-polar solvents

NASA Astrophysics Data System (ADS)

Jadżyn, J.; Żywucki, B.

1986-07-01

cis-trans Conformation of the imide group in propionimide (C 2H 5CONHCOC 2H 5) leads to its cyclic dimerization via the NH⋯OC hydrogen bonds. Dielectric and IR studies in non-polar solvents showed that the dipole moment of the propionimide cyclic dimer is equal to zero. The thermodynamic parameters describing the process of this dimerization are given.

Well-Known Mediators of Selective Oxidation with Unknown Electronic Structure: Metal-Free Generation and EPR Study of Imide-N-oxyl Radicals.

PubMed

Krylov, Igor B; Kompanets, Mykhailo O; Novikova, Katerina V; Opeida, Iosip O; Kushch, Olga V; Shelimov, Boris N; Nikishin, Gennady I; Levitsky, Dmitri O; Terent'ev, Alexander O

2016-01-14

Nitroxyl radicals are widely used in chemistry, materials sciences, and biology. Imide-N-oxyl radicals are subclass of unique nitroxyl radicals that proved to be useful catalysts and mediators of selective oxidation and CH-functionalization. An efficient metal-free method was developed for the generation of imide-N-oxyl radicals from N-hydroxyimides at room temperature by the reaction with (diacetoxyiodo)benzene. The method allows for the production of high concentrations of free radicals and provides high resolution of their EPR spectra exhibiting the superhyperfine structure from benzene ring protons distant from the radical center. An analysis of the spectra shows that, regardless of the electronic effects of the substituents in the benzene ring, the superhyperfine coupling constant of an unpaired electron with the distant protons at positions 4 and 5 of the aromatic system is substantially greater than that with the protons at positions 3 and 6 that are closer to the N-oxyl radical center. This is indicative of an unusual character of the spin density distribution of the unpaired electron in substituted phthalimide-N-oxyl radicals. Understanding of the nature of the electron density distribution in imide-N-oxyl radicals may be useful for the development of commercial mediators of oxidation based on N-hydroxyimides.

Adhesive Properties of Cured Phenylethynyl Containing Imides

NASA Technical Reports Server (NTRS)

Jensen, Brian J.; Chang, Alice C.

1997-01-01

Considerable attention has been directed towards acetylene terminated oligomers over the last 20 years' and recent work has focused on phenylethynyl terminated imide (PETI) oligomers. These reactive oligomers possess several features which make them attractive candidates for use as composite matrices and adhesives. The phenylethynyl group can be readily incorporated into many different functionalized oligomers. The reactive oligomers possess relatively low melt viscosities and thermally cure without the evolution of volatile by-products. Once cured, they typically display high glass transition temperatures (Tgs), excellent solvent resistance and high mechanical properties. new modified phenylethynyl-terminated imide (LaRC MPEI) oligomers were synthesized at various molecular weights utilizing a small amount of trifunctional amine. As long as the amount of triamine is relatively small, this approach produces a mixture of linear, star-shaped and branched polymer chains that has lower melt and solution viscosity than an equivalent molecular weight linear phenylethynyl terminated imide oligomers. The work reported herein involves the synthesis and characterization of a copolymer using this approach and the preparation of blends utilizing a phenylethynyl containing reactive plasticizer of lower molecular weight called LaRC LV-121. The chemistry and properties of this new MPEI as well as some blends of MPEI with LV-121, are presented and compared to the linear version, LARC-PETI-5.

Observation and modeling of mixing-layer development in HED blast-wave-driven shear flow

NASA Astrophysics Data System (ADS)

di Stefano, Carlos

2013-10-01

This talk describes work exploring the sensitivity to initial conditions of hydrodynamic mixing-layer growth due to shear flow in the high-energy-density regime. This work features an approach in two parts, experimental and theoretical. First, an experiment, conducted at the OMEGA-60 laser facility, seeks to measure the development of such a mixing layer. This is accomplished by placing a layer of low-density (initially of either 0.05 or 0.1 g/cm3, to vary the system's Atwood number) carbon foam against a layer of higher-density (initially 1.4 g/cm3) polyamide-imide that has been machined to a nominally-flat surface at its interface with the foam. Inherent roughness of this surface's finish is precisely measured and varied from piece to piece. Ten simultaneous OMEGA beams, comprising a 4.5 kJ, 1-ns pulse focused to a roughly 1-mm-diameter spot, irradiate a thin polycarbonate ablator, driving a blast wave into the foam, parallel to its interface with the polyamide-imide. The ablator is framed by a gold washer, such that the blast wave is driven only into the foam, and not into the polyamide-imide. The subsequent forward motion of the shocked foam creates the desired shear effect, and the system is imaged by X-ray radiography 35 ns after the beginning of the driving laser pulse. Second, a simulation is performed, intending to replicate the flow observed in the experiment as closely as possible. Using the resulting simulated flow parameters, an analytical model can be used to predict the evolution of the mixing layer, as well as track the motion of the fluid in the experiment prior to the snapshot seen in the radiograph. The ability of the model to predict growth of the mixing layer under the various conditions observed in the experiment is then examined. This work is funded by the Predictive Sciences Academic Alliances Program in NNSA-ASC via grant DEFC52- 08NA28616, by the NNSA-DS and SC-OFES Joint Program in High-Energy-Density Laboratory Plasmas, grant number DE-NA0001840, and by the National Laser Use.

Constitutive Models for the Viscoelastic Behavior of Polyimide Membranes at Room and Deep Cryogenic Temperatures

DOE PAGES

Bhandarkar, Suhas; Betcher, Jacob; Smith, Ryan; ...

2016-06-30

Targets for ICF shots on NIF typically use ~500nm thin polyimide films with a coating of 25nm of aluminum as windows that seal the laser entrance hole or LEH. Their role is to contain the hohlraum gas and minimize the extraneous infra-red radiation getting in. This is necessary to precisely control the hohlraum thermal environment for layering inside the capsule with solid deuterium-tritium at 18K. Here, we use our empirical data on the bulging behavior of these foils under various different conditions to develop models to capture the complex viscoelastic behavior of these films at both ambient and cryogenic temperatures.more » The constitutive equations derived from these models give us the ability to quantitatively specify the film’s behavior during the fielding of these targets and set the best parameters for new target designs.« less

Thermoplastic polyimide NEW-TPI (trademark)

NASA Technical Reports Server (NTRS)

Hou, Tan-Hung; Reddy, Rakasi M.

1990-01-01

Thermal and rheological properties of a commercial thermoplastic polyimide, NEW-TPI (trademark), were characterized. The as-received material possesses initially a transient crystallite form with a bimodal distribution in peak melting temperatures. After the melting of the initial crystallite structure, the sample can be recrystallized by various thermal treatments. A bimodal or single modal melting peak distribution is formed for annealing temperatures below or above 360 C, respectively. The recrystallized crystallinities are all transient in nature. The polymers are unable to be recrystallized after being subjected to elevated temperature annealing above 450 C. The recrystallization mechanism was postulated, and a simple kinetics model was found to describe the behavior rather satisfactory under the conditions of prolonged thermal annealing. Rheological measurements made in the linear viscoelastic range support the evidence observed in the thermal analysis. Furthermore, the measurements sustain the manufacturer's recommended processing window of 400 to 420 C for this material.

Understanding the Effect of the Dianhydride Structure on the Properties of Semiaromatic Polyimides Containing a Biobased Fatty Diamine

PubMed Central

2017-01-01

In this work we report the effect of the hard block dianhydride structure on the overall properties of partially biobased semiaromatic polyimides. For the study, four polyimides were synthesized using aliphatic fatty dimer diamine (DD1) as the soft block and four different commercially available aromatic dianhydrides as the hard block: 4,4′-(4,4′-isopropylidenediphenoxy) bis(phthalic anhydride) (BPADA), 4,4′-oxidiphthalic anhydride (ODPA), 4,4′-(Hexafluoroisopropylidene) diphthalic anhydride (6FDA), and 3,3′,4,4′-biphenyltetracarboxylic dianhydride (BPDA). The polymers synthesized were fully organo-soluble thermoplastic branched polyimides with glass transition temperatures close to room temperature. The detailed analysis took into account several aspects of the dianhydrides structure (planarity, rigidity, bridging group between the phtalimides, and electronic properties) and related them to the results obtained by differential scanning calorimetry, rheology, fluorescence and broadband dielectric spectroscopy. Moreover, the effects of physical parameters (crystallization and electronic interactions) on the relaxation behavior are discussed. Despite the presence of the bulky branched soft block given by the dimer diamine, all polyimides showed intermolecular charge transfer complexes, whose extent depends on the electronic properties of the dianhydride hard block. Furthermore, the results showed that polyimides containing flexible and bulky hard blocks turned out fully amorphous while the more rigid dianhydride (BPDA) led to a nanophase separated morphology with low degree of crystallinity resulting in constrained segmental relaxation with high effect on its mechanical response with the annealing time. This work represents the first detailed report on the development and characterization of polyimides based on a biobased fatty dimer diamine. The results highlight the potential of polymer property design by controlled engineering of the aromatic dianhydride blocks. PMID:29333351

Synthesis of polyimides from α,αʹ-bis(3-aminophenoxy)-p-xylene: Spectroscopic, single crystal XRD and thermal studies

NASA Astrophysics Data System (ADS)

Ashraf, Ahmad Raza; Akhter, Zareen; Simon, Leonardo C.; McKee, Vickie; Castel, Charles Dal

2018-05-01

The meta-catenated ether-based diamine monomer α,αʹ-bis(3-aminophenoxy)-p-xylene (3APX) was synthesized from dinitro precursor α,αʹ-bis(3-nitrophenoxy)-p-xylene (3NPX). FTIR, 1H and 13C NMR spectroscopic studies accompanied by elemental analysis were performed for structural elucidations of 3NPX and 3APX. The spatial orientations of 3APX were explored by single crystal X-ray diffraction analysis. Its crystal system was found to be monoclinic, adopting the space group P21/c. The synthesized diamine monomer (3APX) was used for preparation of new series of polyimides by reacting with three different dianhydrides (BTDA, ODPA, 6FDA). The relevant copolyimides were developed via incorporation of 4,4ʹ-methylenedianiline (MDA) in the backbone of afore-synthesized polyimides. The structures of polyimides and copolyimides were verified by FTIR and 1H NMR spectroscopic techniques. Their properties were evaluated by dynamic and isothermal TGA (nitrogen and air atmospheres) and WAXRD studies. Polyimides displayed significantly high thermal stability as their degradation started around 400 °C and it was improved further by execution of copolymerization strategy with MDA. The 5% weight loss temperature (T5) of polyimides under nitrogen atmosphere was in the range of 425-460 °C while for copolyimides it increased to 454-498 °C. Thermal decomposition in air was slower than nitrogen between 400 and 550 °C however it was accelerated above 550 °C. Isothermal TGA disclosed that copolyimides have the ability to endure elevated temperatures for extended period. WAXRD analysis showed the amorphous nature of polyimides and copolyimides.

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.

Slotted Polyimide-Aerogel-Filled-Waveguide Arrays

NASA Technical Reports Server (NTRS)

Rodriguez-Solis, Rafael A.; Pacheco, Hector L.; Miranda, Felix A.; Meador, Mary Ann B.

2013-01-01

This presentation discussed the potential advantages of developing Slotted Waveguide Arrays using polyimide aerogels. Polyimide (PI) aerogels offer great promise as an enabling technology for lightweight aerospace antenna systems. PI aerogels are highly porous solids possessing low density and low dielectric permittivity combined with good mechanical properties. For slotted waveguide array applications, there are significant advantages in mass that more than compensate for the slightly higher loss of the aerogel filled waveguide when compared to state of practice commercial waveguide.

Formulation and characterization of polyimide resilient foams of various densities for aircraft seating applications

NASA Technical Reports Server (NTRS)

Gagliani, J.; Lee, R.; Sorathia, U. A. K.

1981-01-01

Light weight, heat and fire resistant low smoke generating polyimide foams are developed for aircraft seating applications. The material is upgraded and classified into groups for fabrication of cushions possessing acceptable comfort properties. Refinement and selection of foaming processes using a variety of previously developd foaming techniques and definition of property relationships to arrive at the selection and classfication of polyimide foams into five groups in accordance with predetermined ILD values are emphasized.

The effect of simulated low earth orbit radiation on polyimides (UV degradation study)

NASA Technical Reports Server (NTRS)

Forsythe, John S.; George, Graeme A.; Hill, David J. T.; Odonnell, James H.; Pomery, Peter J.; Rasoul, Firas A.

1995-01-01

UV degradation of polyimide films in air and vacuum were studied using UV-visible, ESR, FTIR, and XPS spectroscopies. The UV-visible spectra of polyimide films showed a blue shift in the absorption compared to Kapton. This behavior was attributed to the presence of bulky groups and kinks along the polymer chains which disrupt the formation of a charge transfer complex. The UV-visible spectra showed also that UV irradiation of polyimides result extensively in surface degradation, leaving the bulk of the polymer intact. ESR spectra of polyimides irradiated in vacuum revealed the formation of stable carbon-centered radicals which give a singlet ESR spectrum, while polyimides irradiated in air produced an asymmetric signal shifted to a lower magnetic field, with a higher g value and line width. This signal was attributed to oxygen-cenetered radicals of peroxy and/or alkoxy type. The rate of radical formation in air was two fold higher than for vacuum irradiation, and reached a plateau after a short time. This suggests a continuous depletion of radicals on the surface via an ablative degradation process. FTIR, XPS, and weight loss studies supported this postulate. An XPS study of the surface indicated a substantial increase in the surface oxidation after irradiation in air. The sharp increase in the C-O binding energy peak relative to the C-C peak was believed to be associated with an aromatic ring opening reaction.

Shelf Life of PMR Polyimide Monomer Solutions and Prepregs Extended

NASA Technical Reports Server (NTRS)

Alston, William B.; Scheiman, Daniel A.

2000-01-01

PMR (Polymerization of Monomeric Reactants) technology was developed in the mid-1970's at the NASA Glenn Research Center at Lewis Field for fabricating high-temperature stable polyimide composites. This technology allowed a solution of polyimide monomers or prepreg (a fiber, such as glass or graphite, impregnated with PMR polyimide monomers) to be thermally cured without the release of volatiles that cause the formation of voids unlike the non-PMR technology used for polyimide condensation type resins. The initial PMR resin introduced as PMR 15 is still commercially available and is used worldwide by aerospace industries as the state-of-the-art resin for high-temperature polyimide composite applications. PMR 15 offers easy composite processing, excellent composite mechanical property retention, a long lifetime at use temperatures of 500 to 550 F, and relatively low cost. Later, second-generation PMR resin versions, such as PMR II 50 and VCAP 75, offer improvements in the upper-use temperature (to 700 F) and in the useful life at temperature without major compromises in processing and property retention but with significant increases in resin cost. Newer versions of nontoxic (non-methylene dianiline) PMR resins, such as BAX PMR 15, offer similar advantages as originally found for PMR 15 but also with significant increases in resin cost. Thus, the current scope of the entire PMR technology available meets a wide range of aeronautical requirements for polymer composite applications.

Rigid-Rod Polyimides

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.; Kinder, James D.; Hull, Diana L.; Youngs, Wiley J.

1996-01-01

Experimental polyimides relatively rigid synthesized in effort to exploit some of advantages of rodlike polymers, while alleviating disadvantages. Polymers used to make colorless fibers and transparent films for optical and electronic application.

Thermal cycling tests on surface-mount assemblies

NASA Astrophysics Data System (ADS)

Jennings, C. W.

1988-03-01

The capability of surface-mount (SM) solder joints to withstand various thermal cycle stresses was evaluated through electrical circuit resistance changes of a test pattern and by visual examination for cracks in the solder after exposure to thermal cycling. The joints connected different electrical components, primarily leadless-chip carriers (LCCs), and printed wiring-board (PWB) pads on different laminate substrates. Laminate compositions were epoxy-glass and polyimide-glass with and without copper/Invar/copper (CIC) inner layers, polyimide-quartz, epoxy-Kevlar, and polyimide-Kevlar. The most resistant joints were between small LCCs (24 and 48 pins) and polyimide-glass laminate with CIC inner layers. Processing in joint formation was found to be an important part of joint resistant. Thermal cycling was varied with respect to both time and temperature. A few resistors, capacitors, and inductors showed opens after 500 30-min cycles between -65 C and 125 C. Appreciable moisture contents were measured for laminate materials, especially those of polyimide-Kevlar after equilibration in 100 percent relative humidity at room temperature. If not removed or reduced, moisture can cause delamination in vapor-phase soldering.

Nuclear Instruments and Methods in Physics Research. Section B; Microstructural Characterization of Semi-Interpenetrating Polymer Networks by Positron Lifetime Spectroscopy

NASA Technical Reports Server (NTRS)

Singh, Jag J.; Pater, Ruth H.; Eftekhari, Abe

1998-01-01

Thermoset and thermoplastic polyimides have complementary physical/mechanical properties. Whereas thermoset polyimides are brittle and generally easier to process, thermoplastic polyimides are tough but harder to process. It is expected that a combination of these two types of polyimides may help produce polymers more suitable for aerospace applications. Semi-Interpenetrating Polymer Networks (S-IPNs) of thermoset LaRC(Trademark)-RP46 and thermoplastic LARC(Trademark)-IA polyimides were prepared in weight percent ratios ranging from 100:0 to 0: 100. Positron lifetime measurements were made in these samples to correlate their free volume features with physical/mechanical properties. As expected, positronium atoms are not formed in these samples. The second life time component has been used to infer the positron trap dimensions. The "free volume" goes through a minimum at about 50:50 ratio, suggesting that S-IPN samples are not merely solid solutions of the two polymers. These data and related structural properties of the S-IPN samples have been discussed in this paper.

Epoxy/Glass and Polyimide (LaRC(TradeMark) PETI-8)/Carbon Fiber Metal Laminates Made by the VARTM Process

NASA Technical Reports Server (NTRS)

Cano, Roberto J.; Loos, Alfred C.; Jensen, Brian J.; Britton, Sean M.; Tuncol, Goker; Long, Kai

2010-01-01

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 the potential to reduce the manufacturing cost of composite structures. Fiber metal laminates (FML) made via this process with aluminum, glass fabric, and epoxy resins have been previously fabricated at LaRC. In this work, the VARTM process has been refined for epoxy/glass FMLs and extended to the fabrication of FM Ls with titanium/carbon fabric layers and a polyimide system developed at NASA, LARC(TradeMark) PETI-8. Resin flow pathways were introduced into the titanium foils to aid the infiltration of the polyimide resin. Injection temperatures in the range of 250-280 C were required to achieve the necessary VARTM viscosities (<10 Poise). Laminate quality and initial mechanical properties will be presented.

Development of LaRC (TM): IA thermoplastic polyimide coated aerospace wiring

NASA Technical Reports Server (NTRS)

Keating, Jack

1995-01-01

NASA Langley has invented LaRC(exp TM) IA and IAX which are thermoplastic polyimides with good melting, thermal and chemical resistance properties. It was the objective of this contract to prepare and extrude LaRC (exp TM) polyimide onto aircraft wire and evaluate the polymers performance in this critical application. Based on rheology and chemical resistance studies at Imitec, LaRC (exp TM) IAX melts readily in an extruder, facilitating the manufacture of thin wall coatings. The polyimide does not corode the extruder, develop gel particles nor advance in viscosity. The insulated wire was tested according to MiL-W-22759E test specifications. The resulting wire coated with LaRC (exp TM) IAX displayed exceptional properties: surface resistance, non blocking, non burning, hot fluid resistance, impulse dielectric, insulation resistance, low temperature flexibility, thermal aging, wire weight, dimensions, negligible high temperature shrinkage and stripability. The light weight and other properties merit its application in satellites, missiles and aircraft applications. The extruded IAX results in a polyimide aircraft insulation without seams, outstanding moisture resistance, continuous lengths and abrasion resistance.

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.

Coarse-Grained and Atomistic Modeling of Polyimides

NASA Technical Reports Server (NTRS)

Clancy, Thomas C.; Hinkley, Jeffrey A.

2004-01-01

A coarse-grained model for a set of three polyimide isomers is developed. Each polyimide is comprised of BPDA (3,3,4,4' - biphenyltetracarboxylic dianhydride) and one of three APB isomers: 1,3-bis(4-aminophenoxy)benzene, 1,4-bis(4-aminophenoxy)benzene or 1,3-bis(3-aminophenoxy)benzene. The coarse-grained model is constructed as a series of linked vectors following the contour of the polymer backbone. Beads located at the midpoint of each vector define centers for long range interaction energy between monomer subunits. A bulk simulation of each coarse-grained polyimide model is performed with a dynamic Monte Carlo procedure. These coarsegrained models are then reverse-mapped to fully atomistic models. The coarse-grained models show the expected trends in decreasing chain dimensions with increasing meta linkage in the APB section of the repeat unit, although these differences were minor due to the relatively short chains simulated here. Considerable differences are seen among the dynamic Monte Carlo properties of the three polyimide isomers. Decreasing relaxation times are seen with increasing meta linkage in the APB section of the repeat unit.

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.

Surface Texturing of Polyimide Composite by Micro-Ultrasonic Machining

NASA Astrophysics Data System (ADS)

Qu, N. S.; Zhang, T.; Chen, X. L.

2018-03-01

In this study, micro-dimples were prepared on a polyimide composite surface to obtain the dual benefits of polymer materials and surface texture. Micro-ultrasonic machining is employed for the first time for micro-dimple fabrication on polyimide composite surfaces. Surface textures of simple patterns were fabricated successfully with dimple depths of 150 μm, side lengths of 225-425 μm, and area ratios of 10-30%. The friction coefficient of the micro-dimple surfaces with side lengths of 325 or 425 μm could be increased by up to 100% of that of non-textured surfaces, alongside a significant enhancement of wear resistance. The results show that surface texturing of polyimide composite can be applied successfully to increase the friction coefficient and reduce wear, thereby contributing to a large output torque.

Electrically conductive polyimide film containing gold (III) ions, composition, and process of making

NASA Technical Reports Server (NTRS)

Caplan, Maggie L. (Inventor); Stoakley, Diane M. (Inventor); St. Clair, Anne K. (Inventor)

1996-01-01

An electrically conductive, thermooxidatively stable poltimide, especially a film thereof, is prepared from an intimate admixture of a particular polyimide and gold (III) ions, in an amount sufficient to provide between 17 and 21 percent by weight of gold (III) ions, based on the weight of electrically conductive, thermooxidatively stable polyimide. The particular polyimide is prepared from a polyamic acid which has been synthesized from a dianhydride/diamine combination selected from the group consisting of 3,3',4,4'-benzophenonetetracarboxylic dianhydride and 2,2-bis[4-(4 -aminophenoxy)phenyl]hexafluoropropane; 3,3',4,4'-benzophenonetetracarboxylic dianhydride and 4,4'-oxydianiline; 2,2'-bis(3,4-dicarboxyphenyl)hexafluoropropane dianhydride and 4,4'-oxydianiline; and 3,3'4,4'-benzophenonetetracarboxylic dianhydride and 2,2-bis(3-aminophenyl)hexafluoropropane.

PMR polyimides from solutions containing mixed endcaps

NASA Technical Reports Server (NTRS)

Delvigs, P.

1985-01-01

Previous studies have shown that partial substitution of p-aminostyrene (PAS) for the monomethylester of endo-5-norbornene-2, 3-dicarboxylic acid (NE) lowered the cure temperature of PMR polyimides from 316 to 260 C, but the modified PMR polyimides required higher compression-molding pressures than state-of-the-art PMR-15. In this study PMR polyimides are prepared employing three encaps: NE, PAS, and endo-N-phenyl-5-norbornene-2,3-dicarboximide (PN). The effect of PN addition on the processing characteristics and glass transition temperatures of graphite fiber-reinforced PMR composites is studied. The room temperature and short-time 316 C mechanical properties of the composites are determined. The weight loss and mechanical property retention characteristics of the composites after exposure in air at 316 C are also determined.

Polyimides Derived from Novel Asymmetric Benzophenone Dianhydrides

NASA Technical Reports Server (NTRS)

Chuang, Chun-Hua (Inventor)

2015-01-01

This invention relates to the composition and processes for preparing thermoset polyimides derived from an asymmetric dianhydride, namely 2,3,3',4'-benzophenone dianhydride (a-BTDA) with at least one diamine, and a monofunctional terminal endcaps. The monofunctional terminating groups include 4-phenylethynylphthalic anhydride ester-acid derivatives, phenylethyl trimellitic anhydride (PETA) and its ester derivatives as well as 3-phenylethynylaniline. The process of polyimide composite comprises impregnating monomer reactants of dianhydride or its ester-acid derivatives, diamine and with monofunctional reactive endcaps into glass, carbon, quartz or synthetic fibers and fabrics, and then stack up into laminates and subsequently heated to between 150-375.degree. C. either at atmosphere or under pressure to promote the curing and crosslinking of the reactive endcaps to form a network of thermoset polyimides.

Reliability of spring interconnects for high channel-count polyimide electrode arrays

NASA Astrophysics Data System (ADS)

Khan, Sharif; Ordonez, Juan Sebastian; Stieglitz, Thomas

2018-05-01

Active neural implants with a high channel-count need robust and reliable operational assembly for the targeted environment in order to be classified as viable fully implantable systems. The discrete functionality of the electrode array and the implant electronics is vital for intact assembly. A critical interface exists at the interconnection sites between the electrode array and the implant electronics, especially in hybrid assemblies (e.g. retinal implants) where electrodes and electronics are not on the same substrate. Since the interconnects in such assemblies cannot be hermetically sealed, reliable protection against the physiological environment is essential for delivering high insulation resistance and low defusibility of salt ions, which are limited in complexity by current assembly techniques. This work reports on a combination of spring-type interconnects on a polyimide array with silicone rubber gasket insulation for chronically active implantable systems. The spring design of the interconnects on the backend of the electrode array compensates for the uniform thickness of the sandwiched gasket during bonding in assembly and relieves the propagation of extrinsic stresses to the bulk polyimide substrate. The contact resistance of the microflex-bonded spring interconnects with the underlying metallized ceramic test vehicles and insulation through the gasket between adjacent contacts was investigated against the MIL883 standard. The contact and insulation resistances remained stable in the exhausting environmental conditions.

Effect of stabilization temperature during pyrolysis process of P84 co-polyimide-based tubular carbon membrane for H2/N2 and He/N2 separations

NASA Astrophysics Data System (ADS)

Sazali, N.; Salleh, W. N. W.; Ismail, A. F.; Ismail, N. H.; Aziz, F.; Yusof, N.; Hasbullah, H.

2018-04-01

In this study, the effect of stabilization temperature on the performance of tubular carbon membrane was being investigated. P84 co-polyimide-based tubular carbon membrane will be fabricated through the dip-coating technique. The tubular carbon membrane performance can be controlled by manipulating the pyrolysis conditions which was conducted at different stabilization temperatures of 250, 300, 350, 400, and 450°C under N2 environment (200 ml/min). The prepared membranes were characterized by using scanning electron microscopy (SEM), x-ray diffraction (XRD), and pure gas permeation system. The pure gas of H2, He, and N2 were used to determine the permeation properties of the carbon membrane. The P84 co-polyimide-based tubular carbon membrane stabilized at 300°C demonstrated an excellent permeation property with H2, He, and N2 gas permeance of 1134.51±2.87, 1287.22±2.86 and 2.98±1.28GPU, respectively. The highest H2/N2 and He/N2 selectivity of 380.71±2.34 and 431.95±2.61 was obtained when the stabilization temperature of 450°C was applied. It is concluded that the stabilization temperatures have protrusive effect on the carbon membrane properties specifically their pore structure, and eventually their gas separation properties.

Exploiting the acylating nature of the imide-Ugi intermediate: a straightforward synthesis of tetrahydro-1,4-benzodiazepin-2-ones.

PubMed

Mossetti, Riccardo; Saggiorato, Dèsirèe; Tron, Gian Cesare

2011-12-16

We describe a simple and novel protocol for the synthesis of tetrahydro-1,4-benzodiazepin-2-ones with three points of diversity, exploiting the acylating properties of the recently rediscovered Ugi-imide. The final compounds can be easily prepared in three synthetic steps using a multicomponent reaction, a Staudinger reduction, and an acylative protocol, with good to excellent yields for each synthetic step.

1-Ethyl-1-methyl piperidinium bis(trifluoromethanesulfonyl)imide as a co-solvent in Li-ion batteries

NASA Astrophysics Data System (ADS)

Kim, Ketack; Cho, Young-Hyun; Shin, Heon-Cheol

2013-03-01

1-Ethyl-1-methyl piperidinium bis(trifluoromethanesulfonyl)imide (EMP-TFSI) is an ionic liquid with a melting temperature of 85 °C. Although it is a solid salt, it shows good miscibility with carbonate solvents, which allows EMP-TFSI to be used as a co-solvent in these systems. Ethylene carbonate is another solid co-solvent used in Li-ion batteries. Due to its smaller cationic size, EMP-TFSI provides better conductivity as a co-solvent than 1-methyl-1-propyl piperidinium bis(trifluoromethanesulfonyl)imide (MPP-TFSI), which is the smallest room-temperature piperidinium liquid salt known. In cells with 50 wt% IL and 50 wt% carbonate electrolyte, an EMP-TFSI mixed electrolyte performs better than an MPP-TFSI mixed electrolyte. Additionally, the discharge capacity values obtained from rate capability tests carried out with mixed EMP-TFSI are as good as those conducted with a pure carbonate electrolyte.

Distinct molecular structures and hydrogen bond patterns of α,α-diethyl-substituted cyclic imide, lactam, and acetamide derivatives in the crystalline phase

NASA Astrophysics Data System (ADS)

Krivoshein, Arcadius V.; Ordonez, Carlos; Khrustalev, Victor N.; Timofeeva, Tatiana V.

2016-10-01

α,α-Dialkyl- and α-alkyl-α-aryl-substituted cyclic imides, lactams, and acetamides show promising anticonvulsant, anxiolytic, and anesthetic activities. While a number of crystal structures of various α-substituted cyclic imides, lactams, and acetamides were reported, no in-depth comparison of crystal structures and solid-state properties of structurally matched compounds have been carried out so far. In this paper, we report molecular structure and intermolecular interactions of three α,α-diethyl-substituted compounds - 3,3-diethylpyrrolidine-2,5-dione, 3,3-diethylpyrrolidin-2-one, and 2,2-diethylacetamide - in the crystalline phase, as studied using single-crystal X-ray diffraction and IR spectroscopy. We found considerable differences in the patterns of H-bonding and packing of the molecules in crystals. These differences correlate with the compounds' melting points and are of significance to physical pharmacy and formulation development of neuroactive drugs.

Imide Oligomers Endcapped with Phenylethynl Phthalic Anhydrides and Polymers Therefrom

NASA Technical Reports Server (NTRS)

Hergenrother, Paul M. (Inventor); Smith, Joseph G., Jr. (Inventor)

1998-01-01

Controlled molecular weight phenylethynyl terminated imide oligomers (PETIs) have been prepared by the cyclodehydration of precursor phenylethynyl terminated amic acid oligomers. Amino terminated amic acid oligomers are prepared from the reaction of dianhydride(s) with an excess of diamine(s) and subsequently endcapped with phenylethynyl phthalic anhydride(s) (PEPA). The polymerizations are carried out in polar aprotic solvents such as N-methyl-2-pyrrolidinone or N.N-dimethylacetamide under nitrogen at room temperature. The amic acid oligomers are subsequently cyclodehydrated either thermally or cheznicauy to the corresponding imide oligomers. Direct preparation of PETIs from the reaction of dianhydxide(s) with an excess of diamine(s) and endcapped with phenylethynyl phthalic anhydride(s) has been performed in m-cresol. Phenylethynyl phthalic anhydrides are synthesized by the palladium catalyzed reaction of phenylacetylene with bromo substituted phthalic anhydrides in triethylamine. These new materials exhibit excellent properties and are potentially useful as adhesives, coatings, films, moldings and composite matrices.

Imide oligomers endcapped with phenylethynyl phthalic anhydrides and polymers therefrom

NASA Technical Reports Server (NTRS)

Hergenrother, Paul M. (Inventor); Smith, Jr., Joseph G. (Inventor)

1996-01-01

Controlled molecular weight phenylethynyl terminated imide oligomers (PETIs) have been prepared by the cyclodehydration of precursor phenylethynyl terminated amic acid oligomers. Amino terminated amic acid oligomers are prepared from the reaction of dianhydride(s) with an excess of diamine(s) and subsequently endcapped with phenylethynyl phthalic anhydride(s) (PEPA). The polymerizations are carried out in polar aprotic solvents such as N-methyl-2-pyrrolidinone or N,N-dimethylacetamide under nitrogen at room temperature. The amic acid oligomers are subsequently cyclodehydrated either thermally or chemically to the corresponding imide oligomers. Direct preparation of PETIs from the reaction of dianhydride(s) with an excess of diamine(s) and endcapped with phenylethynyl phthalic anhydride(s) has been performed in m-cresol. Phenylethynyl phthalic anhydrides are synthesized by the palladium catalyzed reaction of phenylacetylene with bromo substituted phthalic anhydrides in triethylamine. These new materials exhibit excellent properties and are potentially useful as adhesives, coatings, films, moldings and composite matrices.

Measurement of Microscale Bio-Thermal Responses by Means of a Micro-Thermocouple Probe

DTIC Science & Technology

2001-10-25

3) A silane coupler (VM-652, HD MicroSystems) was applied as a primer for good adhesion of the polyimide coating (Pyralin® PI2556, HD...MicroSystems), which was used as an insulating layer. We also used SiO2 instead of polyimide . (4) A gold (Au) thin film was deposited by means of the ion...sputtering technique. (5) A coating of polyimide /SiO2 was applied. (6) Finally, a coating of MPC (2-methacryloyloxyethyl phosphorylcholine) copolymers

Dielectric Properties of Piezoelectric Polyimides

NASA Technical Reports Server (NTRS)

Ounaies, Z.; Young, J. A.; Simpson, J. O.; Farmer, B. L.

1997-01-01

Molecular modeling and dielectric measurements are being used to identify mechanisms governing piezoelectric behavior in polyimides such as dipole orientation during poling, as well as degree of piezoelectricity achievable. Molecular modeling on polyimides containing pendant, polar nitrile (CN) groups has been completed to determine their remanent polarization. Experimental investigation of their dielectric properties evaluated as a function of temperature and frequency has substantiated numerical predictions. With this information in hand, we are then able to suggest changes in the molecular structures, which will then improve upon the piezoelectric response.