Hybrid copper complex-derived conductive patterns printed on polyimide substrates

NASA Astrophysics Data System (ADS)

Lee, Byoungyoon; Jeong, Sooncheol; Kim, Yoonhyun; Jeong, Inbum; Woo, Kyoohee; Moon, Jooho

2012-06-01

We synthesized new copper complexes that can be readily converted into highly conductive Cu film. Mechanochemical milling of copper (I) oxide suspended in formic acid resulted in the submicron-sized Cu formate together Cu nanoparticles. The submicrometer-sized Cu formates are reactive toward inter-particle sintering and metallic Cu seeds present in the Cu complexes assist their decomposition and the nucleation of Cu. The hybrid copper complex film printed on polyimide substrate is decomposed into dense and uniform Cu layer after annealing at 250 °C for 30 min under nitrogen atmosphere. The resulting Cu film exhibited a low resistivity of 8.2 μΩ·cm and good adhesion characteristics.

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.

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.

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

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

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

2016-05-18

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

Exploration of photosensitive polyimide as the modification layer in thin film microcircuit

NASA Astrophysics Data System (ADS)

Liu, Lily; Song, Changbin; Xue, Bin; Li, Jing; Wang, Junxi; Li, Jinmin

2018-02-01

Positive type photosensitive polyimide is used as the modification layer in the thin film transistors production process. The photosensitive polyimide is not only used as the second insulating layer, it can also be used instead of a mask because of the photosensitivity. A suitable curing condition can help photosensitive polyimide form the high performance polyimide with orderly texture inside, and the performance of imidization depends on the precise control of temperature, time, and heat control during the curing process. Therefore, experiments of different stepped up heating tests are made, and the ability of protecting silicon dioxide is analyzed.

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.

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.

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.

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.

Adhesive evaluation of new polyimides

NASA Technical Reports Server (NTRS)

Stclair, Terry L.; Progar, Donald J.

1987-01-01

During the past 10 to 15 years, the Materials Division at NASA Langley Research Center (LaRC) has developed several novel high temperature polyimide adhesives for anticipated needs of the aerospace industry. These developments have resulted from fundamental studies of structure-property relationships in polyimides. Recent research at LaRC has involved the synthesis and evaluation of copolyimides which incorporate both flexibilizing bridging groups and meta-linked benzene rings. The purpose was to develop systems based on low cost, readily available monomers. Two of these copolyimides evaluated as adhesives for bonding titanium alloy, Ti(6Al-4V), are identified as LARC-STPI and STPI-LARC-2. Lap shear strength (LSS) measurements were used to determine the strength and durability of the adhesive materials. LSS results are presented for LARC-TPI and LARC-STPI lap shear specimens thermally exposed in air at 232 C for up to 5000 hrs. LARC-TPI was shown to perform better than the copolymer LARC-STPI which exhibited poor thermooxidative performance possibly due to the amines used which would tend to oxidize easier than the benzophenone system in LARC-TPI.

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.

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.

Studies on the oxidation of hexamethylbenzene 2: Preparation of dimethylpyromellitic acid

NASA Technical Reports Server (NTRS)

Chiba, K.; Tomura, S.

1986-01-01

Hexamethylbenzene (HMB) was difficult to be oxidized with an alkaline potassium permanganate solution, since HMB was insoluble in an aqueous alkaline solution. But, when HMB was warmed with 50% nitric acid for a short time, and then treated with aqueous potassium permanganate, the reaction occurred readily and dimethylpyromellitic acid was obtained. When HMB was warmed with 50% nitric acid for 1 to 2 minutes, a yellow material was produced, which was soluble in hot aqueous potassium hydroxide, though free from carboxylic acids. It contained a little amount of bis-(nitromethyl)prehnitene and several unknown compounds. Further, the heat stability of polyimide prepared by the reaction of tetramethyldimethylpyromellitate with 4,4 prime-diaminodiphenylmethane turned out to be nearly equal to that of polyimide prepared from tetramethylpyromellitate.

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.

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.

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.

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.

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

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.

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.

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.

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.

Manufacturing processes for fabricating graphite/PMR 15 polyimide structural elements

NASA Technical Reports Server (NTRS)

Sheppard, C. H.; Hoggatt, J. T.; Symonds, W. A.

1979-01-01

Investigations were conducted to obtain commercially available graphite/PMR-15 polyimide prepreg, develop an autoclave manufacturing process, and demonstrate the process by manufacturing structural elements. Controls were established on polymer, prepreg, composite fabrication, and quality assurance, Successful material quality control and processes were demonstrated by fabricating major structural elements including flat laminates, hat sections, I beam sections, honeycomb sandwich structures, and molded graphite reinforced fittings. Successful fabrication of structural elements and simulated section of the space shuttle aft body flap shows that the graphite/PMR-15 polyimide system and the developed processes are ready for further evaluation in flight test hardware.

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.

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.

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.

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.

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.

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.

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.

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.

Bonded polyimide fuel cell package

DOEpatents

Morse, Jeffrey D.; Jankowski, Alan; Graff, Robert T.; Bettencourt, Kerry

2010-06-08

Described herein are processes for fabricating microfluidic fuel cell systems with embedded components in which micron-scale features are formed by bonding layers of DuPont Kapton.TM. polyimide laminate. A microfluidic fuel cell system fabricated using this process is also described.

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.

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

NASA Technical Reports Server (NTRS)

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

1980-01-01

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

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.

Polyimide Composites from 'Salt-Like' Solution Precursors

NASA Technical Reports Server (NTRS)

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

2001-01-01

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

PMR polyimides: Processable high temperature composite matrix resins

NASA Technical Reports Server (NTRS)

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

1975-01-01

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

PMR polyimides - Processable high temperature composite matrix resins

NASA Technical Reports Server (NTRS)

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

1975-01-01

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

Tailor making high performance graphite fiber reinforced PMR polyimides

NASA Technical Reports Server (NTRS)

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

1974-01-01

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

New polyimide polymer has excellent processing characterisitcs with improved thermo-oxidative and hydrolytic stabilities

NASA Technical Reports Server (NTRS)

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

1972-01-01

Polyimide P10P and its processing technique apply to most high temperature plastic products, devices and castings. Prepolymer, when used as varnish, impregnates fibers directly and is able to be processed into advanced composities. Material may also be used as molding powder and adhesive.

Tough, processable simultaneous semi-interpenetrating polyimides

NASA Technical Reports Server (NTRS)

Pater, Ruth H. (Inventor)

1996-01-01

A high temperature semi-interpenetrating polymer network (semi-IPN) was developed which had significantly improved processability, damage tolerance and mechanical performance, when compared to the commercial Thermid.RTM. materials. This simultaneous semi-IPN was prepared by mixing a thermosetting polyimide with a thermoplastic monomer precursor solution (NR-15082) and allowing them to react upon heating. This reaction occurs at a rate which decreases the flow and broadens the processing window. Upon heating at a higher temperature, there is an increase in flow. Because of the improved flow properties, broadened processing window and enhanced toughness, high strength polymer matrix composites, adhesives and molded articles can now be prepared from the acetylene endcapped polyimides which were previously inherently brittle and difficult to process.

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.

Amorphous silicon and organic thin film transistors for electronic applications

NASA Astrophysics Data System (ADS)

Zhou, Lisong

Recently, flexible thin film electronics has attracted huge research interest, and as now, many prototypes are being developed and demonstrated by companies around the world, including displays, logic circuit, and solar cells. Flexible electronics offers many potential advantages: it can not only generate new functions like flexible displays or solar cells, also allow very low cost manufacturing through the use of cheap polymeric substrates and roll-to-roll fabrication. a-Si:H TFT fabrications are compatible with flexible polyimide substrate materials. With the interests in the space environment, for the first time, we tested the performance changes of flexible a-Si:H TFTs, on polyimide substrates, due to irradiation and mechanical stress. Significant changes were found on TFTs after irradiation with fast electrons, which, however, was essentially removed by post-irradiation thermal annealing. On the other hand, few changes were found in TFTs by mechanical stress. These preliminary results indicate that it can be readily engineered for space applications. Furthermore, for the first time, we designed and fabricated ungated n+ muC-Si and gated a-Si:H strain sensors on flexible polyimide substrates. Compared with commercial metallic foil strain sensors, ungated muC-Si sensors and gated a-Si:H sensors are two orders of magnitude smaller in area and consume two orders or magnitude less power. Integration with a-Si:H TFTs can also allow large arrays of strain sensors to be fabricated. To take advantage of lower glass-transition-temperature polymeric substrate materials, reduced processing temperature is desired. The 150°C low-temperature deposition process is achieved by using hydrogen dilution in the PECVD process. The TFT performance and bias stability property are tested similar to that of a 250°C process. These results suggest its viability for practical applications. For even lower process temperature, we have considered organic TFTs. As a practical demonstration, we integrated pentacene TFTs with OLEDs in a simple display. Pentacene TFT passivation techniques were researched, and a PVA and parylene bilayer structure was used. We designed and demonstrated 48 x 48-pixel active matrix OTFTOLED displays, and to our best knowledge, they are the largest on glass substrates and the first on flexible PET substrates. Device performance, uniformity and stability are also compared. These results demonstrate that pentacene TFTs are viable candidates for active-matrix OLED displays and other flexible electronics applications.

Bonded polyimide fuel cell package and method thereof

DOEpatents

Morse, Jeffrey D.; Jankowski, Alan; Graff, Robert T.; Bettencourt, Kerry

2005-11-01

Described herein are processes for fabricating microfluidic fuel cell systems with embedded components in which micron-scale features are formed by bonding layers of DuPont Kapton.TM. polyimide laminate. A microfluidic fuel cell system fabricated using this process is also described.

Method of preparation of bonded polyimide fuel cell package

DOEpatents

Morse, Jeffrey D [Martinez, CA; Jankowski, Alan [Livermore, CA; Graff, Robert T [Modesto, CA; Bettencourt, Kerry [Dublin, CA

2011-04-26

Described herein are processes for fabricating microfluidic fuel cell systems with embedded components in which micron-scale features are formed by bonding layers of DuPont Kapton.TM. polyimide laminate. A microfluidic fuel cell system fabricated using this process is also described.

Better End-Cap Processing for Oxidation-Resistant Polyimides

NASA Technical Reports Server (NTRS)

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

2004-01-01

A class of end-cap compounds that increase the thermo-oxidative stab ility of polyimides of the polymerization of monomeric reactants (PM R) type has been extended. In addition, an improved processing proto col for this class of end-cap compounds has been invented.

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.

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.

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.

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.

Tough, processable simultaneous semi-interpenetrating polyimides

NASA Technical Reports Server (NTRS)

Pater, Ruth H. (Inventor)

1994-01-01

A high temperature semi-interpenetrating polymer network (semi-IPN) was developed which had significantly improved processability, damage tolerance, and mechanical performance when compared to the commercial Thermid materials. This simultaneous semi-IPN was prepared by mixing a thermosetting polyimide with a thermoplastic monomer precursor solution (NR150B2) and allowing them to react upon heating. This reaction occurs at a rate which decreases the flow and broadens the processing window. Upon heating at a higher temperature, there is an increase in flow. Because of the improved flow properties, broadened processing window and enhanced toughness, high strength polymer matrix composites, adhesives and molded articles can now be prepared from the acetylene endcapped polyimides which were previously inherently brittle and difficult to process.

Tackifier for addition polyimides containing monoethylphthalate

NASA Technical Reports Server (NTRS)

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

1981-01-01

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

Polyimides 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.

Develop, demonstrate, and verify large area composite structural bonding with polyimide adhesives. [adhesively bonding graphite-polyimide structures

NASA Technical Reports Server (NTRS)

Bhombal, B. D.; Wykes, D. H.; Hong, K. C.; Stenersen, A. A.

1982-01-01

The technology required to produce graphite-polyimide structural components with operational capability at 598 K (600 F) is considered. A series of polyimide adhesives was screened for mechanical and physical properties and processibility in fabricating large midplane bonded panels and honeycomb sandwich panels in an effort to fabricate a structural test component of the space shuttle aft body flap. From 41 formulations, LaRC-13, FM34B-18, and a modified LaRC-13 adhesive were selected for further evaluation. The LaRC-13 adhesive was rated as the best of the three adhesives in terms of availability, cost, processibility, properties, and ability to produce void fee large area (12" x 12") midplane bonds. Surface treatments and primers for the adhesives were evaluated and processes were developed for the fabrication of honeycomb sandwich panels of very good quality which was evidenced by rupture in the honeycomb core rather than in the facesheet bands on flatwise tensile strength testing. The fabrication of the adhesively bonded honeycomb sandwich cover panels, ribs, and leading edge covers of Celion graphite/LARC-160 polyimide laminates is described.

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.

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.

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.

Automated Solvent Seaming of Large Polyimide Membranes

NASA Technical Reports Server (NTRS)

Rood, Robert; Moore, James D.; Talley, Chris; Gierow, Paul A.

2006-01-01

A solvent-based welding process enables the joining of precise, cast polyimide membranes at their edges to form larger precise membranes. The process creates a homogeneous, optical-quality seam between abutting membranes, with no overlap and with only a very localized area of figure disturbance. The seam retains 90 percent of the strength of the parent material. The process was developed for original use in the fabrication of wide-aperture membrane optics, with areal densities of less than 1 kg/m2, for lightweight telescopes, solar concentrators, antennas, and the like to be deployed in outer space. The process is just as well applicable to the fabrication of large precise polyimide membranes for flat or inflatable solar concentrators and antenna reflectors for terrestrial applications. The process is applicable to cast membranes made of CP1 (or equivalent) polyimide. The process begins with the precise fitting together and fixturing of two membrane segments. The seam is formed by applying a metered amount of a doped solution of the same polyimide along the abutting edges of the membrane segments. After the solution has been applied, the fixtured films are allowed to dry and are then cured by convective heating. The weld material is the same as the parent material, so that what is formed is a homogeneous, strong joint that is almost indistinguishable from the parent material. The success of the process is highly dependent on formulation of the seaming solution from the correct proportion of the polyimide in a suitable solvent. In addition, the formation of reliable seams depends on the deposition of a precise amount of the seaming solution along the seam line. To ensure the required precision, deposition is performed by use of an automated apparatus comprising a modified commercially available, large-format, ink-jet print head on an automated positioning table. The printing head jets the seaming solution into the seam area at a rate controlled in coordination with the movement of the positioning table.

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.

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)

1994-01-01

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.

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.

Retractable Sun Shade

NASA Technical Reports Server (NTRS)

Frank, A.; Derespinis, S. F.; Mockovciak, John, Jr.

1986-01-01

Window-shade type spring roller contains blanket, taken up by rotating cylindrical frame and held by frame over area to be shaded. Blanket made of tough, opaque polyimide material. Readily unfurled by mechanism to protect space it encloses from Sun. Blanket forms arched canopy over space and allows full access to it from below. When shading not needed, retracted mechanism stores blanket compactly. Developed for protecting sensitive Space Shuttle payloads from direct sunlight while cargo-bay doors open. Adapted to shading of greenhouses, swimming pools, and boats.

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.

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.

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

NASA Technical Reports Server (NTRS)

Cano, Robert J.; Jensen, Brian J.

2013-01-01

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

Structural-modification mechanism for polyimide-doped poly(tetrafluoroethylene)at subthreshold fluences using 248 nm radiation

NASA Astrophysics Data System (ADS)

Davis, C. R.; Snyder, R. W.; Egitto, F. D.; D'Couto, G. C.; Babu, S. V.

1994-09-01

Single-photon excimer laser ablation of neat poly(tetrafluoroethylene) (PTFE) is not observed at emissions in the 'quartz' UV, i.e., from about 190-380 nm. However, it has been successfully demonstrated that, when the fluoropolymer is doped with small quantities of polyimide (PI), ablation in the quartz UV, e.g., at 248 and 308 nm and pulse widths of about 25 ns, is readily achieved. When PI-PTFE blends are exposed to subthreshold fluences, considerable changes in surface topography occur although clearly defined structures, e.g., pits, are not formed. Using photoacoustic infrared spectroscopy to evaluate surface and bulk chemical changes to blends exposed to subthreshold excimer laser fluences, is less than 100 mJ/sq cm, it is shown that PI (1) is distributed throughout the bulk and resides at the surface and (2) is selectively absorbing the high-energy photons and as a result being preferentially removed from the surface.

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.

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.

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.

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.

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.

Solvent resistant thermoplastic aromatic poly(imidesulfone) and process for preparing same

NASA Technical Reports Server (NTRS)

St.clair, T. L.; Yamaki, D. A. (Inventor)

1983-01-01

A process for preparing a thermoplastic poly(imidesulfone) is disclosed. This resulting material has thermoplastic properties which are generally associated with polysulfones but not polyimides, and solvent resistance which is generally associated with polyimides but not polysulfones. This system is processable in the 250 to 350 C range for molding, adhesive and laminating applications. This unique thermoplastic poly(imidesulfone) is obtained by incorporating an aromatic sulfone moiety into the backbone of an aromatic linear polyimide by dissolving a quantity of a 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA) in a solution of 3,3'-diaminodiphenylsulfone and bis(2-methoxyethyl)ether, precipitating the reactant product in water, filtering and drying the recovered poly(amide-acid sulfone) and converting it to the poly(imidesulfone) by heating.

Process for preparing solvent resistant, thermoplastic aromatic poly(imidesulfone)

NASA Technical Reports Server (NTRS)

St.clair, T. L.; Yamaki, D. A. (Inventor)

1984-01-01

A process for preparing a thermoplastic poly(midesulfone) is disclosed. This resulting material has thermoplastic properties which are generally associated with polysulfones but not polyimides, and solvent resistant which is generally associated with polyimides but not polysulfones. This system is processable in the 250 to 350 C range for molding, adhesive and laminating applications. This unique thermoplastic poly(imidesulfone) is obtained by incorporating an aromatic sulfone moiety into the backbone of an aromatic linear polyimide by dissolving a quantity of a 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA) in a solution of 3,3'-diaminodiphenylsulfone and bis(2-methoxyethyl)ether, precipitating the reactant product in water, filtering and drying the recovered poly(amide-acid sulfone) and converting it to the poly(imidesulfone) by heating.

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.

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.

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.

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.

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

NASA Technical Reports Server (NTRS)

1980-01-01

A quality assurance program was developed which included specifications for celion/LARC-160 polyimide materials and quality control of materials and processes. The effects of monomers and/or polymer variables and prepeg variables on the processibility of celion/LARC prepeg were included. Processes for fabricating laminates, honeycomb core panels, and chopped fiber moldings were developed. Specimens and conduct tests were fabricated to qualify the processes for fabrication of demonstration components.

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.

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.

Enhanced performance of solution-processed organic thin-film transistors with a low-temperature-annealed alumina interlayer between the polyimide gate insulator and the semiconductor.

PubMed

Yoon, Jun-Young; Jeong, Sunho; Lee, Sun Sook; Kim, Yun Ho; Ka, Jae-Won; Yi, Mi Hye; Jang, Kwang-Suk

2013-06-12

We studied a low-temperature-annealed sol-gel-derived alumina interlayer between the organic semiconductor and the organic gate insulator for high-performance organic thin-film transistors. The alumina interlayer was deposited on the polyimide gate insulator by a simple spin-coating and 200 °C-annealing process. The leakage current density decreased by the interlayer deposition: at 1 MV/cm, the leakage current densities of the polyimide and the alumina/polyimide gate insulators were 7.64 × 10(-7) and 3.01 × 10(-9) A/cm(2), respectively. For the first time, enhancement of the organic thin-film transistor performance by introduction of an inorganic interlayer between the organic semiconductor and the organic gate insulator was demonstrated: by introducing the interlayer, the field-effect mobility of the solution-processed organic thin-film transistor increased from 0.35 ± 0.15 to 1.35 ± 0.28 cm(2)/V·s. Our results suggest that inorganic interlayer deposition could be a simple and efficient surface treatment of organic gate insulators for enhancing the performance of solution-processed organic thin-film transistors.

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.

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.

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.

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.

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

NASA Technical Reports Server (NTRS)

Hou, Tan-Hung

2014-01-01

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

Thermoplastic polymides and composites therefrom

NASA Technical Reports Server (NTRS)

Harris, Frank W. (Inventor)

1994-01-01

A new class polyimide and polyimide precursors based on diaryl oxyalkylene diamines, such as 1,3-bis[4-aminophenoxy]-2,2-dimethyl propane, a process for their preparation and their use as the continuous phase for the manufacture of composites and composite laminates reinforced by reinforcing agents such as carbon fibers, Kevlar.TM., and other similar high strength reinforcing agents. The polyimides and molecular composites obtained from the diamines according to the invention show thermoplastic properties, excellent flex fatigue and fracture resistance, and excellent thermal and oxidative stability.

Isomer effects on polyimide properties

NASA Technical Reports Server (NTRS)

Stump, B. L.

1975-01-01

Polyimide polymers which are thermally stable and processable are developed. The addition of alkyl substituents to an aromatic ring in the polymer backbone is examined along with polyimide precursor amines containing functional groups that allow for post-cure crosslinking. The synthesis of key monomers is reported, including 2,4,6-tris (m-aminobenzyl) 1,3,5-trimethyl benzene and 2,4,6-tris (p-aminobenzyl) 1,3,5-trimethyl benzene. The preparation of a key monomer, 2,5,3-triamino benzophenone, is reported.

Tackifier for addition polyimides

NASA Technical Reports Server (NTRS)

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

1980-01-01

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

Modified LaRC(TM)-IA Polyimides

NASA Technical Reports Server (NTRS)

St. Clair, Terry L.; Chang, Alice C.; Hou, Tan H.; Working, Dennis C.

1994-01-01

Modified versions of thermoplastic polyimide LaRC(TM)-IA incorporate various amounts of additional, rigid moieties into backbones of LaRC(TM)-IA molecules. Modified versions more resistant to solvents and exhibit higher glass-transition temperatures, yet retain melt-flow processability of unmodified LaRC(TM)-IA.

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

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.

1999-01-01

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

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

NASA Technical Reports Server (NTRS)

Pater, Ruth H.

1990-01-01

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

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

NASA Technical Reports Server (NTRS)

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

1986-01-01

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

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.

Polyimide from bis(n-isoprenyl)s of aryl diamides

NASA Technical Reports Server (NTRS)

Smith, Joseph G., Jr. (Inventor); Ottenbrite, Raphael M. (Inventor)

1993-01-01

A process and polyimide product formed by the reaction of a bismaleimide with a bis(amidediene) is disclosed wherein the bis(amidediene) is formed by reacting an excess of an acid chloride with 1,4-N,N'-diisoprenyl 2,3,5,6-tetramethy1 benzene.

Resin/graphite fiber composites

NASA Technical Reports Server (NTRS)

Cavano, P. J.

1974-01-01

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

Development of autoclave moldable addition-type polyimides

NASA Technical Reports Server (NTRS)

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

1976-01-01

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

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.

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

NASA Technical Reports Server (NTRS)

Merlette, J. B.

1972-01-01

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

An Approach to Processable Polyimides

NASA Technical Reports Server (NTRS)

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

1999-01-01

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

Low-void polyimide resins for autoclave processing

NASA Technical Reports Server (NTRS)

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

1972-01-01

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

Industry technology assessment of graphite-polymide composite materials. [conferences

NASA Technical Reports Server (NTRS)

1975-01-01

An assessment of the current state of the art and the future prospects for graphite polyimide composite material technology is presented. Presentations and discussions given at a minisymposium of major issues on the present and future use, availability, processing, manufacturing, and testing of graphite polyimide composite materials are summarized.

Polyimide Prepregs With Improved Tack

NASA Technical Reports Server (NTRS)

Vanucci, R.

1987-01-01

Drape and tack improved without loss of strength. Composites made with PMR-15 (or equivalent) polyimides have gained acceptance as viable engineering materials for high-use-temperature applications. Acceptance due to both thermo-oxidative stability of PMR-15 (or equivalent) and ease which PMR-15 (or equivalent) prepreg materials processed into composite structures.

Development and demonstration of manufacturing processes for fabricating graphite/LARC 160 polyimide structural elements

NASA Technical Reports Server (NTRS)

Frost, R. K.; Jones, J. S.; Dynes, P. J.; Wykes, D. H.

1981-01-01

The development and demonstration of manufacturing technologies for the structural application of Celion graphite/LARC-160 polyimide composite material is discussed. Process development and fabrication of demonstration components are discussed. Process development included establishing quality assurance of the basic composite material and processing, nondestructive inspection of fabricated components, developing processes for specific structural forms, and qualification of processes through mechanical testing. Demonstration components were fabricated. The demonstration components consisted of flat laminates, skin/stringer panels, honeycomb panels, chopped fiber compression moldings, and a technology demonstrator segment (TDS) representative of the space shuttle aft body flap.

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.

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.

Processing for maximizing the level of crystallinity in linear aromatic polyimides

NASA Technical Reports Server (NTRS)

St.clair, Terry L. (Inventor)

1991-01-01

The process of the present invention includes first treating a polyamide acid (such as LARC-TPI polyamide acid) in an amide-containing solvent (such as N-methyl pyrrolidone) with an aprotic organic base (such as triethylamine), followed by dehydrating with an organic dehydrating agent (such as acetic anhydride). The level of crystallinity in the linear aromatic polyimide so produced is maximized without any degradation in the molecular weight thereof.

Annihilation of photochemical reactivity of photo-alignment layer.

PubMed

Hong, S H; Hwang, Y J; Lee, S G; Shin, D M

2008-09-01

The gas-polymer and liquid-polymer interfacial reactions of photosensitive polyimide can annihilate photo-reactive carbon-carbon double bonds, which remain after photo-alignment process. The annihilation processes dramatically affect voltage holding ratio and reorientation of photo-active functional groups. Photochemical dimerizations were identified using UV-visible and FT-IR spectroscopy. Polyimide films containing cinnamate groups were irradiated by linear polarized ultra violet (LPUV) light. Schadt et al. claims that the photo-alignment results from the anisotropy depletion of the cinnamate side chains as a consequence of the (2+2) cycloaddition reactions. The photo-aligned polyimide induces the orientation of nematic liquid crystals perpendicular to the polarization axis. However, the un-reacted photo-sensitive functional groups generate problems such as image sticking and reduced contrast ratio. Voltage holding ratio and photo-fading observed from photo-alignment layer can be dramatically improved by annihilation process of remnant photoreactive groups.

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.

The surface properties of fluorinated polyimides exposed to VUV and atomic oxygen

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

The effect of atomic oxygen flux and VUV radiation alone and in combination on the surface of fluorinated polyimide films was studied using XPS spectroscopy. Exposure of fluorinated polyimides to VUV radiation alone caused no observable damage to the polymer surface, while an atomic oxygen flux resulted in substantial oxidation of the surface. On the other hand, exposure to VUV radiation and atomic oxygen in combination caused extensive oxidation of the polymer surface after only 2 minutes of exposure. The amount of oxidized carbon on the polymer surface indicated that there is aromatic ring opening oxidation. The changes in the O1s/C1s, N1s/C1s, and F1s/C1s ratios suggested that an ablative degradation process is highly favorable. A synergistic effect of VUV radiation in the presence of atomic oxygen is clearly evidenced from the XPS study. The atomic oxygen could be considered as the main factor in the degradation process of fluorinated polyimide films exposed to a low earth orbit environment.

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.

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

NASA Technical Reports Server (NTRS)

1981-01-01

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

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.

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.

Polyimide Resins Resist Extreme Temperatures

NASA Technical Reports Server (NTRS)

2009-01-01

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

Fabrication of polydimethylsiloxane (PDMS) - based multielectrode array for neural interface.

PubMed

Kim, Jun-Min; Oh, Da-Rong; Sanchez, Joaquin; Kim, Shang-Hyub; Seo, Jong-Mo

2013-01-01

Flexible multielectrode arrays (MEAs) are being developed with various materials, and polyimide has been widely used due to the conveniece of process. Polyimide is developed in the form of photoresist. And this enable precise and reproducible fabrication. PDMS is another good candidate for MEA base material, but it has poor surface energy and etching property. In this paper, we proposed a better fabrication process that could modify PDMS surface for a long time and open the site of electrode and pad efficiently without PDMS etching.

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

NASA Technical Reports Server (NTRS)

Petker, I.; Segimoto, M.

1973-01-01

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

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

NASA Technical Reports Server (NTRS)

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

1991-01-01

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

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.

Space Environmentally Durable Polyimides and Copolyimides

NASA Technical Reports Server (NTRS)

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

2006-01-01

Polyimides displaying low color in thin films, atomic oxygen resistance, vacuum ultraviolet radiation resistance, solubility in organic solvents in the imide form, high glass transition (T(sub g)) temperatures, and high thermal stability are provided. The poly(amide acid)s, copoly(amide acid)s, polyimides and copolyimides are prepared by the reaction of stoichiometric ratios of an aromatic &anhydride with diamines which contain phenylphosphine oxide groups in polar aprotic solvents. Controlled molecular weight oligomeric (amide acid)s and imides can be prepared by offsetting the stoichiometry according to the Carothers equation using excess diamine and endcapping with aromatic anhydrides. The polyimide materials can be processed into various material forms such as thin films, fibers, foams, threads, adhesive film, coatings, dry powders, and fiber coated prepreg, and uses include thin film membranes on antennas, second-surface mirrors, thermal optical coatings, and multilayer thermal insulation (MLI) blanket materials.

Space Environmentally Durable Polyimides and Copolyimides

NASA Technical Reports Server (NTRS)

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

2005-01-01

Polyimides displaying low color in thin films, atomic oxygen resistance, vacuum ultraviolet radiation resistance, solubility in organic solvents in the imide form, high glass transition (T(sub g)) temperatures, and high thermal stability are provided. The poly(amide acid)s, copoly(amide acid)s, polyimides and copolyimides are prepared by the reaction of stoichiometric ratios of an aromatic dianhydride with diamines which contain phenylphosphine oxide groups in polar aprotic solvents. Controlled molecular weight oligomeric (amide acid)s and imides can be prepared by offsetting the stoichiometry according to the Carothers equation using excess diamine and endcapping with aromatic anhydrides The polyimide materials can be processed into various material forms such as thin films, fibers, foams, threads, adhesive film, coatings, dry powders, and fiber coated prepreg, and uses include thin film membranes on antennas, second-surface mirrors, thermal optical coatings, and multilayer thermal insulation (MLI) blanket materials.

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

NASA Technical Reports Server (NTRS)

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

1975-01-01

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

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

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

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

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

NASA Technical Reports Server (NTRS)

Alston, W. B.

1985-01-01

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

Optimal Substrate Preheating Model for Thermal Spray Deposition of Thermosets onto Polymer Matrix Composites

NASA Technical Reports Server (NTRS)

Ivosevic, M.; Knight, R.; Kalidindi, S. R.; Palmese, G. R.; Tsurikov, A.; Sutter, J. K.

2003-01-01

High velocity oxy-fuel (HVOF) sprayed, functionally graded polyimide/WC-Co composite coatings on polymer matrix composites (PMC's) are being investigated for applications in turbine engine technologies. This requires that the polyimide, used as the matrix material, be fully crosslinked during deposition in order to maximize its engineering properties. The rapid heating and cooling nature of the HVOF spray process and the high heat flux through the coating into the substrate typically do not allow sufficient time at temperature for curing of the thermoset. It was hypothesized that external substrate preheating might enhance the deposition behavior and curing reaction during the thermal spraying of polyimide thermosets. A simple analytical process model for the deposition of thermosetting polyimide onto polymer matrix composites by HVOF thermal spray technology has been developed. The model incorporates various heat transfer mechanisms and enables surface temperature profiles of the coating to be simulated, primarily as a function of substrate preheating temperature. Four cases were modeled: (i) no substrate preheating; (ii) substrates electrically preheated from the rear; (iii) substrates preheated by hot air from the front face; and (iv) substrates electrically preheated from the rear and by hot air from the front.

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

NASA Technical Reports Server (NTRS)

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

1985-01-01

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

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.

Investigations on effect of laser-induced self-assembled patterning on optical properties of flexible polyimide substrates for solar cell applications

NASA Astrophysics Data System (ADS)

Shukla, Ashish K.; Yadav, Vinayak M.; Kumar, Akash; Palani, I. A.; Manivannan, Anbarasu

2018-01-01

Polyimide (PI) offers promising features such as high strength and excellent thermal stability for flexible solar panels. The flexible solar cell demands maximum absorption of solar insolation through stacked layers to enhance its performance. However, the fluorescence emission (FE) in inactive polyimide substrate hinders the absorption of irradiated solar energy. In this research work, an attempt has been made to generate rippled morphology on PI substrate using laser processing that enhances the absorption and moderates the FE. These changes are confirmed by calculating the Urbach energy (Eu) of the rippled structure, which is found to be 2.5 times that of the pristine substrate. Furthermore, to reduce the FE, tungsten (W) was coated on the rippled structure of the laser-processed PI, and a significant reduction of 70% FE is achieved compared to the FE of unprocessed PI. These enhanced characteristics of PI obtained by laser processing will be highly helpful for improving the overall performance of flexible solar cells.

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.

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.

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).

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.

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.

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.

Tough high performance composite matrix

NASA Technical Reports Server (NTRS)

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

1994-01-01

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

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

NASA Technical Reports Server (NTRS)

2005-01-01

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

High Performance Polymers and Composites (HiPPAC) Center

NASA Technical Reports Server (NTRS)

Mintz, Eric A.; Veazie, David

2005-01-01

NASA University Research Centers funding has allowed Clark Atlanta University (CAU) to establish a High Performance Polymers and Composites (HiPPAC) Research Center. Clark Atlanta University, through the HiPPAC Center has consolidated and expanded its polymer and composite research capabilities through the development of research efforts in: (1) Synthesis and characterization of polymeric NLO, photorefractive, and piezoelectric materials; (2) Characterization and engineering applications of induced strain smart materials; (3) Processable polyimides and additives to enhance polyimide processing for composite applications; (4) Fabrication and mechanical characterization of polymer based composites.

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

NASA Technical Reports Server (NTRS)

Chuang, CHun-Hua (Inventor)

2006-01-01

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

New High Temperature Cross Linking Monomers

NASA Technical Reports Server (NTRS)

Scola, Daniel A.

1978-01-01

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

A tough high performance composite matrix

NASA Technical Reports Server (NTRS)

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

1992-01-01

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

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.

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.

Processable polyimide adhesive and matrix composite resin

NASA Technical Reports Server (NTRS)

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

1990-01-01

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

Atomic-Oxygen Effects on POSS Polyimides in Low Earth Orbit

DTIC Science & Technology

2012-01-11

one. Figure 2. Reaction scheme for the synthesis of the N-[(hepta-isobutylPOSS) propyl ]-3,5- diaminobenzamide monomer used to prepare side-chain (SC...atomic oxygen. Earlier results from laboratory- and space-based studies are given, as well as new information on the synthesis and in-space...methods.39,40 Polyimide synthesis and processing was pioneered by workers at Dupont in the 1950’s, with Kapton being the first commercially

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.

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

NASA Technical Reports Server (NTRS)

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

1972-01-01

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

Mechanical properties of three layer glass fibre reinforced unsaturated polyester filled with P84 Polyimide

NASA Astrophysics Data System (ADS)

Ibrahim, Nik Noor Idayu Nik; Mamauod, Siti Nur Liyana; Romli, Ahmad Zafir

2017-12-01

The glass fibre reinforced orthophthalic unsaturated polyester composite was widely used in the pipeline industry as a replacement to the corroded steel pipes. A filler which possesses high mechanical performance at high temperature; P84 Polyimide used as the particulate reinforcement in the unsaturated polyester matrix system to increase the mechanical performance of the glass fibre reinforced unsaturated polyester. The glass fibre composite laminates were prepared through a hand lay-up technique and fabricated into three layer laminate. Prior to be used as the matrix system in the lamination process, the unsaturated polyester resin was mixed with masterbatch P84 Polyimide at three loadings amount of 1, 3, and 5 wt%. The addition of P84 Polyimide at 1, 3, and 5 wt% increased the tensile properties and flexural properties especially at 1 wt% filler loading. As the filler loading increased, the tensile properties and flexural properties showed decreasing pattern. In the dynamic mechanical analysis, the values of storage modulus were taken at two points; 50 °C and 150 °C which were the storage modulus before and after the glass transition temperature. All storage modulus showed fluctuation trend for both before and after Tg. However, the storage modulus of the filled composite laminates after Tg showed higher values than unfilled composite laminates at all filler loading. Since the P84 Polyimide possesses high thermal stability, the presence of P84 Polyimide inside the composite system had assisted in delaying the Tg. In terms of the filler dispersion, the Cole-Cole plot showed an imperfect semi-circular shape which indicated good filler dispersion.

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.

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.

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.

Molecular relaxations, molecular orientation, and the friction characteristics of polyimide films. [wear characteristics of polymeric lubricant

NASA Technical Reports Server (NTRS)

Fusaro, R. L.

1975-01-01

The friction characteristics of polyimide films bonded to metallic substrates were studied from 25 to 500 C. These results were interpreted in terms of molecular orientation and thermomechanical data obtained by torsional braid analysis (TBA). A large friction transition was found to occur at 40 + or - 10 C in a dry argon atmosphere (10 ppm H2O). It was postulated that the mechanical stresses of sliding transform or reorder the molecules on the surface into a configuration conducive to easy shear, such as an extended chain. The molecular relaxation which occurs in this temperature region appears to give the molecules the necessary freedom for this reordering process to occur. The effects of velocity, reversibility, and thermal prehistory on the friction properties of polyimide were also studied.

Molecular relaxations, molecular orientation and the friction characteristics of polyimide films

NASA Technical Reports Server (NTRS)

Fusaro, R. L.

1975-01-01

The friction characteristics of polyimide films bonded to metallic substrates were studied from 25 to 500 C. These results were interpreted in terms of molecular orientation and thermomechanical data obtained by torsional braid analysis (TBA). A large friction transition was found to occur at 40 plus or minus 10 C in a dry argon atmosphere (10 ppm H2O). It was postulated that the mechanical stresses of sliding transform or reorder the molecules on the surface into a configuration conducive to easy shear, such as an extended chain. The molecular relaxation which occurs in this temperature region appears to give the molecules the necessary freedom for this reordering process to occur. The effects of velocity, reversibility, and thermal prehistory on the friction properties of polyimide were also studied.

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

NASA Astrophysics Data System (ADS)

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

2017-06-01

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

Elastomer toughened polyimide adhesives

NASA Technical Reports Server (NTRS)

St.clair, A. K.; St.clair, T. L. (Inventor)

1983-01-01

A rubber-toughened addition-type polyimide composition is disclosed which has excellent high temperature bonding characteristics in the fully cured state, and improved peel strength and adhesive fracture resistance physical property characteristics. The process for making the improved adhesive involves preparing the rubber containing amic acid prepolymer by chemically reacting an amine-terminated elastomer and an aromatic diamine with an aromatic dianhydride with which a reactive chain stopper anhydride was mixed, and utilizing solvent or mixture of solvents for the reaction.

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

NASA Technical Reports Server (NTRS)

Pater, Ruth H. (Inventor)

1992-01-01

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

Recent developments in polyimide and bismaleimide adhesives

NASA Technical Reports Server (NTRS)

Politi, R. E.

1985-01-01

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

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.

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.

3D Printing All-Aromatic Polyimides using Mask-Projection Stereolithography: Processing the Nonprocessable.

PubMed

Hegde, Maruti; Meenakshisundaram, Viswanath; Chartrain, Nicholas; Sekhar, Susheel; Tafti, Danesh; Williams, Christopher B; Long, Timothy E

2017-08-01

High-performance, all-aromatic, insoluble, engineering thermoplastic polyimides, such as pyromellitic dianhydride and 4,4'-oxydianiline (PMDA-ODA) (Kapton), exhibit exceptional thermal stability (up to ≈600 °C) and mechanical properties (Young's modulus exceeding 2 GPa). However, their thermal resistance, which is a consequence of the all-aromatic molecular structure, prohibits processing using conventional techniques. Previous reports describe an energy-intensive sintering technique as an alternative technique for processing polyimides with limited resolution and part fidelity. This study demonstrates the unprecedented 3D printing of PMDA-ODA using mask-projection stereolithography, and the preparation of high-resolution 3D structures without sacrificing bulk material properties. Synthesis of a soluble precursor polymer containing photo-crosslinkable acrylate groups enables light-induced, chemical crosslinking for spatial control in the gel state. Postprinting thermal treatment transforms the crosslinked precursor polymer to PMDA-ODA. The dimensional shrinkage is isotropic, and postprocessing preserves geometric integrity. Furthermore, large-area mask-projection scanning stereolithography demonstrates the scalability of 3D structures. These unique high-performance 3D structures offer potential in fields ranging from water filtration and gas separation to automotive and aerospace technologies. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Toughening of thermosetting polyimides

NASA Technical Reports Server (NTRS)

Gollob, D. S.; Mandell, J. F.; Mcgarry, F. J.

1979-01-01

Work directed toward increasing the resistance to crack propagation of thermoset polyimides is described. Rubber modification and Teflon microfiber impregnation techniques for increasing fracture toughness are investigated. Unmodified Kerimid 601 has a fracture surface work value of 0.20 in-lbs/sq in. Dispersed particles of amine terminated butadiene acrylonitrile liquid rubber or of silicone rubber do not raise this value much. By contrast, 5 percent of well fibrillated Teflon produces an eight-fold increase in fracture toughness. Further process improvements should increase this factor to 20-30.

Dispersion of Single Wall Carbon Nanotubes by in situ Polymerization Under Sonication

NASA Technical Reports Server (NTRS)

Park, Cheol; Ounaies, Zoubeida; Watson, Kent A.; Crooks, Roy E.; Smith, Joseph, Jr.; Lowther, Sharon E.; Connell, John W.; Siochi, Emilie J.; Harrison, Joycelyn S.; St.Clair, Terry L.

2002-01-01

Single wall nanotube reinforced polyimide nanocomposites were synthesized by in situ polymerization of monomers of interest in the presence of sonication. This process enabled uniform dispersion of single wall carbon nanotube (SWNT) bundles in the polymer matrix. The resultant SWNT-polyimide nanocomposite films were electrically conductive (antistatic) and optically transparent with significant conductivity enhancement (10 orders of magnitude) at a very low loading (0.1 vol%). Mechanical properties as well as thermal stability were also improved with the incorporation of the SWNT.

Validation of a Polyimide Foam Model for Use in Transmission Loss Applications

NASA Technical Reports Server (NTRS)

Hong, Kwanwoo; Bolton, J. Stuart; Cano, Roberto J.; Weiser, Erik S.; Jensen, Brian J.; Silcox, Rich; Howerton, Brian M.; Maxon, John; Wang, Tongan; Lorenzi, Tyler

2010-01-01

The work described in this paper was focused on the use of a new polyimide foam in a double wall sound transmission loss application. Recall that polyimide foams are functionally attractive, compared to polyurethane foams, for example, owing to their fire resistance. The foam considered here was found to have a flow resistivity that was too high for conventional acoustical applications, and as a result, it was processed by partial crushing to lower the flow resistivity into an acceptable range. Procedures for measuring the flow resistivity and Young s modulus of the material have been described, as was an inverse characterization procedure for estimating the remaining Biot parameters based on standing wave tube measurements of transmission loss and absorption coefficient. The inverse characterization was performed using a finite element model implementation of the Biot poro-elastic material theory. Those parameters were then used to predict the sound transmission loss of a double panel system lined with polyimide foam, and the predictions were compared with full-scale transmission loss measurements. The agreement between the two was reasonable, especially in the high and low frequency limits; however, it was found that the SEA model resulted in an under-prediction of the transmission loss in the mid-frequency range. Nonetheless, it was concluded that the performance of polyimide foam could be predicted using conventional poro-elastic material models and that polyimide foam may offer an attractive alternative to other double wall linings in certain situations: e.g., when fire resistance is a key issue. Future work will concentrate on reducing the density of the foam to values similar to those used in current aircraft sidewall treatments, and developing procedures to improve the performance of the foam in transmission loss applications.

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.

Niobium flex cable for low temperature high density interconnects

NASA Astrophysics Data System (ADS)

van Weers, H. J.; Kunkel, G.; Lindeman, M. A.; Leeman, M.

2013-05-01

This work describes the fabrication and characterization of a Niobium on polyimide flex cable suitable for sub-Kelvin temperatures. The processing used can be extended to high density interconnects and allows for direct integration with printed circuit boards. Several key parameters such as RRR, Tc, current carrying capability at 4 K and thermal conductivity in the range from 0.15 to 10 K have been measured. The average Tc was found to be 8.9 K, with a minimum of 8.3 K. Several samples allowed for more than 50 mA current at 4 K while remaining in the superconducting state. The thermal conductivity for this flex design is dominated by the polyimide, in our case Pyralin PI-2611, and is in good agreement with published thermal conductivity data for a polyimide called Upilex R. Registered trademark of Ube Industries, Japan.

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.

Development of High Temperature Type Vacuum Insulation Panel using Soluble Polyimide and Characteristic Evaluation

NASA Astrophysics Data System (ADS)

Araki, Kuninari; Kamoto, Daigorou; Matsuoka, Shin-Ichi

The utilization is expected from the high-insulated characteristic as a tool for energy saving also in the high temperature insulation fields as in vacuum insulation panels (VIP) in the future. For high temperature, the material composition and process of VIP were reviewed, the SUS foil was adopted as packaging material, and soluble polyimide was developed as the thermo compression bonding material for high temperature VIP at 150°C. To lower the glass-transition temperature (Tg) under 200°C, we elaborated the new soluble polyimide using aliphatic diamine copolymer, and controlled Tg to about 176°C. By making from trial VIP and evaluations, it was possible to be maintain high performance concerning the coefficient of thermal conductivity [λ<0.008 W/(m·K) at 150°C].

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.

Stable Polyimides for Terrestrial and Space Uses

NASA Technical Reports Server (NTRS)

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

2005-01-01

Polyimides of a recently developed type have an attractive combination of properties, including low solar absorptivity (manifested as low color) when cast into thin films, resistance to atomic oxygen and ultraviolet radiation, solubility in organic solvents, high glass-transition temperatures, and high thermal stability. The focus of the development work was on polymers that can endure the space environment and that have specific combinations of properties for use on Gossamer spacecraft. Because of their unique combination of properties, these polymers are also expected to find use in a variety of other applications on Earth as well as in space. Examples of other space applications include membranes on antennas, second-surface mirrors, thermal optical coatings, and multilayer thermal insulation. For both terrestrial and space applications, these polyimides can be processed into various forms, including films, fibers, foams, threads, adhesives, and coatings.

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.

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.

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.

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

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.

Integrated manufacturing approach to attain benchmark team performance

NASA Astrophysics Data System (ADS)

Chen, Shau-Ron; Nguyen, Andrew; Naguib, Hussein

1994-09-01

A Self-Directed Work Team (SDWT) was developed to transfer a polyimide process module from the research laboratory to our wafer fab facility for applications in IC specialty devices. The SDWT implemented processes and tools based on the integration of five manufacturing strategies for continuous improvement. These were: Leadership Through Quality (LTQ), Total Productive Maintenance (TMP), Cycle Time Management (CTM), Activity-Based Costing (ABC), and Total Employee Involvement (TEI). Utilizing these management techniques simultaneously, the team achieved six sigma control of all critical parameters, increased Overall Equipment Effectiveness (OEE) from 20% to 90%, reduced cycle time by 95%, cut polyimide manufacturing cost by 70%, and improved its overall team member skill level by 33%.

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

NASA Technical Reports Server (NTRS)

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

1978-01-01

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

A thermoplastic polyimidesulfone. [synthesis of processable and solvent resistant system

NASA Technical Reports Server (NTRS)

St. Clair, T. L.; Yamaki, D. A.

1984-01-01

A polymer system has been prepared which has the excellent thermoplastic properties generally associated with polysulfones, and the solvent resistance and thermal stability of aromatic polyimides. This material, with improved processability over the base polyimide, can be processed in the 260-325 C range in such a manner as to yield high quality, tough unfilled moldings; strong, high-temperature-resistant adhesive bonds; and well consolidated, graphite-fiber-reinforced moldings (composites). The unfilled moldings have physical properties that are similar to aromatic polysulfones which demonstrates the potential as an engineering thermoplastic. The adhesive bonds exhibit excellent retention of initial strength levels even after thermal aging for 5000 hours at 232 C. The graphite-fiber-reinforced moldings have mechanical properties which makes this polymer attractive for the fabrication of structural composites.

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

NASA Technical Reports Server (NTRS)

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

1993-01-01

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

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

NASA Technical Reports Server (NTRS)

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

1984-01-01

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

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

Polyimide-Foam/Aerogel Composites for Thermal Insulation

NASA Technical Reports Server (NTRS)

Williams, Martha; Fesmire, James; Sass, Jared; Smith, Trent; Weoser. Erol

2009-01-01

Composites of specific types of polymer foams and aerogel particles or blankets have been proposed to obtain thermal insulation performance superior to those of the neat polyimide foams. These composites have potential to also provide enhanced properties for vibration dampening or acoustic attenuation. The specific type of polymer foam is denoted "TEEK-H", signifying a series, denoted H, within a family of polyimide foams that were developed at NASA s Langley Research Center and are collectively denoted TEEK (an acronym of the inventors names). The specific types of aerogels include Nanogel aerogel particles from Cabot Corporation in Billerica, MA. and of Spaceloft aerogel blanket from Aspen Aerogels in Northborough, MA. The composites are inherently flame-retardant and exceptionally thermally stable. There are numerous potential uses for these composites, at temperatures from cryogenic to high temperatures, in diverse applications that include aerospace vehicles, aircraft, ocean vessels, buildings, and industrial process equipment. Some low-temperature applications, for example, include cryogenic storage and transfer or the transport of foods, medicines, and chemicals. Because of thermal cycling, aging, and weathering most polymer foams do not perform well at cryogenic temperatures and will undergo further cracking over time. The TEEK polyimides are among the few exceptions to this pattern, and the proposed composites are intended to have all the desirable properties of TEEK-H foams, plus improved thermal performance along with enhanced vibration or acoustic-attenuation performance. A composite panel as proposed would be fabricated by adding an appropriate amount of TEEK friable balloons into a mold to form a bottom layer. A piece of flexible aerogel blanket material, cut to the desired size and shape, would then be placed on the bottom TEEK layer and sandwiched between another top layer of polyimide friable balloons so that the aerogel blanket would become completely encased in an outer layer of TEEK friable balloons. Optionally, the process could be further repeated to produce multiple aerogel-blanket layers interspersed with and encased by TEEK friable balloons.

Considerations Concerning the Development and Testing of In-situ Materials for Martian Exploration

NASA Technical Reports Server (NTRS)

Kim, M.-H. Y.; Heilbronn, L.; Thibeault, S. A.; Simonsen, L. C.; Wilson, J. W.; Chang, K.; Kiefer, R. L.; Maahs, H. G.

2000-01-01

Natural Martian surface materials are evaluated for their potential use as radiation shields for manned Mars missions. The modified radiation fluences behind various kinds of Martian rocks and regolith are determined by solving the Boltzmann equation using NASA Langley s HZETRN code along with the 1977 Solar Minimum galactic cosmic ray environmental model. To make structural shielding composite materials from constituents of the Mars atmosphere and from Martian regolith for Martian surface habitats, schemes for synthesizing polyimide from the Mars atmosphere and for processing Martian regolith/polyimide composites are proposed. Theoretical predictions of the shielding properties of these composites are computed to assess their shielding effectiveness. Adding high-performance polymer binders to Martian regolith to enhance structural properties enhances the shielding properties of these composites because of the added hydrogenous constituents. Laboratory testing of regolith simulant/polyimide composites is planned to validate this prediction.

Thermoplastic copolyimides and composites therefrom

NASA Technical Reports Server (NTRS)

Harris, Frank (Inventor); Gabori, Patricia A. (Inventor)

1994-01-01

Copolyimide compositions and methods for their preparation which are melt-processible at relative low pressures, i.e. less than 1000 psi, and are suited for laminating and molding, are described. The invention additionally encompasses copolyimide precursors, reinforced polyimide composites and laminates made from said polyimides where the composite is reinforced by fibrous materials. This is achieved by reacting at least one aromatic dianhydride where each anhydride group is located on an aromatic ring with the carbonyl units in an ortho orientation relative to one another, with at least one diamine which is capable of a transmidization reaction upon incorporation into the polyimide backbone, and with at least one other diamine which is not capable of undergoing such reaction, the diamine which is capable of undergoing the transimidization reaction being present in an amount of from about 1-50 mole percent in relation to the diamine that is not susceptable to transimidization.

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.

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.

Elastomer toughened polyimide adhesives. [bonding metal and composite material structures for aircraft and spacecraft

NASA Technical Reports Server (NTRS)

St.clair, A. K.; St.clair, T. L. (Inventor)

1985-01-01

A rubber-toughened, addition-type polyimide composition is disclosed which has excellent high temperature bonding characteristics in the fully cured state and improved peel strength and adhesive fracture resistance physical property characteristics. The process for making the improved adhesive involves preparing the rubber-containing amic acid prepolymer by chemically reacting an amine-terminated elastomer and an aromatic diamine with an aromatic dianhydride with which a reactive chain stopper anhydride has been mixed, and utilizing solvent or mixture of solvents for the reaction.

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.

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).

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

NASA Technical Reports Server (NTRS)

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

2004-01-01

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

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

NASA Technical Reports Server (NTRS)

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

2003-01-01

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

Critical Issues for Cu(InGa)Se2 Solar Cells on Flexible Polymer Web

NASA Technical Reports Server (NTRS)

Eser, Erten; Fields, Shannon; Shafarman, William; Birkmire, Robert

2007-01-01

Elemental in-line evaporation on glass substrates has been a viable process for the large-area manufacture of CuInSe2-based photovoltaics, with module efficiencies as high as 12.7% [1]. However, lightweight, flexible CuInSe2-based modules are attractive in a number of applications, such as space power sources. In addition, flexible substrates have an inherent advantage in manufacturability in that they can be deposited in a roll-to-roll configuration allowing continuous, high yield, and ultimately lower cost production. As a result, high-temperature polymers have been used as substrates in depositing CuInSe2 films [2]. Recently, efficiency of 14.1% has been reported for a Cu(InGa)Se2-based solar cell on a polyimide substrate [3]. Both metal foil and polymer webs have been used as substrates for Cu(InGa)Se2-based photovoltaics in a roll-to-roll configuration with reasonable success [4,5]. Both of these substrates do not allow, readily, the incorporation of Na into the Cu(InGa)Se2 film which is necessary for high efficiency devices [3]. In addition, polymer substrates, can not be used at temperatures that are optimum for Cu(InGa)Se2 deposition. However, unlike metal foils, they are electrically insulating, simplifying monolithically-integrated module fabrication and are not a source of impurities diffusing into the growing film. The Institute of Energy Conversion (IEC) has modified its in-line evaporation system [6] from deposition onto glass substrates to roll-to-roll deposition onto polyimide (PI) film in order to investigate key issues in the deposition of large-area Cu(InGa)Se2 films on flexible polymer substrates. This transition presented unexpected challenges that had to be resolved. In this paper, two major problems, spitting from the Cu source and the cracking of Mo back contact film, will be discussed and the solution to each will be presented.

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.

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

NASA Technical Reports Server (NTRS)

Orwoll, Robert A.

1997-01-01

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

A thermoplastic polyimidesulfone

NASA Technical Reports Server (NTRS)

St.clair, T. L.; Yamaki, D. A.

1982-01-01

A polymer system has been prepared which has the excellent thermoplastic properties generally associated with polysulfones, and the solvent resistance and thermal stability of aromatic polyimides. This material, with improved processability over the base polyimide, can be processed in the 260-325 C range in such a manner as to yield high quality, tough unfilled moldings; strong, high-temperature-resistant adhesive bonds; and well consolidated, graphite-fiber-reinforced moldings (composities). The unfilled moldings have physical properties that are similar to aromatic polysulfones which demonstrates the potential as an engineering thermoplastic. The adhesive bonds exhibit excellent retention of initial strength levels even after thermal aging for 5000 hours at 232 C. The graphite-fiber-reinforced moldings have mechanical properties which makes this polymer attractive for the fabrication of structural composites.

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.

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.

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

NASA Technical Reports Server (NTRS)

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

2004-01-01

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

Enhanced adhesion for LIGA microfabrication by using a buffer layer

DOEpatents

Bajikar, Sateesh S.; De Carlo, Francesco; Song, Joshua J.

2004-01-27

The present invention is an improvement on the LIGA microfabrication process wherein a buffer layer is applied to the upper or working surface of a substrate prior to the placement of a resist onto the surface of the substrate. The buffer layer is made from an inert low-Z material (low atomic weight), a material that absorbs secondary X-rays emissions from the substrate that are generated from the substrate upon exposure to a primary X-rays source. Suitable materials for the buffer layer include polyamides and polyimide. The preferred polyimide is synthesized form pyromellitic anhydride and oxydianiline (PMDA-ODA).

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

NASA Technical Reports Server (NTRS)

1996-01-01

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

Titanium reinforced boron-polyimide composite

NASA Technical Reports Server (NTRS)

Clark, G. A.; Clayton, K. I.

1969-01-01

Processing techniques for boron polyimide prepreg were developed whereby composites could be molded under vacuum bag pressure only. A post-cure cycle was developed which resulted in no loss in room temperature mechanical properties of the composite at any time during up to 16 hours at 650 F. A design utilizing laminated titanium foil was developed to achieve a smooth transition of load from the titanium attachment points into the boron-reinforced body of the structure. The box beam test article was subjected to combined bending and torsional loads while exposed to 650 F. Loads were applied incrementally until failure occurred at 83% design limit load.

Flexible amorphous oxide thin-film transistors on polyimide substrate for AMOLED

NASA Astrophysics Data System (ADS)

Xu, Zhiping; Li, Min; Xu, Miao; Zou, Jianhua; Gao, Zhuo; Pang, Jiawei; Guo, Ying; Zhou, Lei; Wang, Chunfu; Fu, Dong; Peng, Junbiao; Wang, Lei; Cao, Yong

2014-10-01

We report a flexible amorphous Lanthanide doped In-Zn-O (IZO) thin-film transistor (TFT) backplane on polyimide (PI) substrate. In order to de-bond the PI film from the glass carrier easily after the flexible AMOLED process, a special inorganic film is deposited on the glass before the PI film is coated. The TFT exhibited a field-effect mobility of 6.97 cm2V-1 s-1, a subthreshold swing of 0.248 V dec-1, and an Ion/Ioff ratio of 5.19×107, which is sufficient to drive the OLEDs.

InN thin-film transistors fabricated on polymer sheets using pulsed sputtering deposition at room temperature

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

Lye, Khe Shin; Kobayashi, Atsushi; Ueno, Kohei

Indium nitride (InN) is potentially suitable for the fabrication of high performance thin-film transistors (TFTs) because of its high electron mobility and peak electron velocity. However, InN is usually grown using a high temperature growth process, which is incompatible with large-area and lightweight TFT substrates. In this study, we report on the room temperature growth of InN films on flexible polyimide sheets using pulsed sputtering deposition. In addition, we report on the fabrication of InN-based TFTs on flexible polyimide sheets and the operation of these devices.

Enhanced adhesion for LIGA microfabrication by using a buffer layer

DOEpatents

Bajikar, Sateesh S.; De Carlo, Francesco; Song, Joshua J.

2001-01-01

The present invention is an improvement on the LIGA microfabrication process wherein a buffer layer is applied to the upper or working surface of a substrate prior to the placement of a resist onto the surface of the substrate. The buffer layer is made from an inert low-Z material (low atomic weight), a material that absorbs secondary X-rays emissions from the substrate that are generated from the substrate upon exposure to a primary X-rays source. Suitable materials for the buffer layer include polyamides and polyimide. The preferred polyimide is synthesized form pyromellitic anhydride and oxydianiline (PMDA-ODA).

Polyimide amic acid salts and polyimide membranes formed therefrom

DOEpatents

Ding, Yong; Bikson, Benjamin; Nelson, Joyce Katz; Macheras, James Timothy

2004-04-06

The invention relates to preparation and uses of novel polymeric materials, polyimide amic acid salts (PIAAS). The use of these materials for the fabrication of fluid separation membranes is further disclosed.

Improvements to the Synthesis of Polyimide Aerogels

NASA Technical Reports Server (NTRS)

Meador, Mary Ann B.; Nguyen, Baochau N.; Guo, Haiquan; Vivod, Stephanie; He, Zuhui; Malow, Ericka; Silva, Rebecca

2011-01-01

Cross-linked polyimide aerogels are viable approach to higher temperature, flexible insulation for inflatable decelerators. Results indicate that the all-polyimide aerogels are as strong or stronger than polymer reinforced silica aerogels at the same density. Currently, examining use of carbon nanofiber and clay nanoparticles to improve performance. Flexible, polyimide aerogels have potential utility in other applications such as space suits, habitats, shelter applications, etc. where low dusting is desired

Development of graphite/polyimide honeycomb core materials

NASA Technical Reports Server (NTRS)

Stone, R. H.

1978-01-01

Honeycomb panel constructions consisting entirely of graphite/polyimide composites were developed and evaluated. Graphite/polyimide composites, were used in the honeycomb core webs and in pre-cured sandwich skins. Polyimide adhesives were also developed and evaluated for use in skin-core bonding. The purpose of this program was to develop light weight sandwich constructions for high temperature applications which could provide comparable shear strength and stiffness to metallic honeycomb constructions.

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.

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.

A flexible insulator of a hollow SiO2 sphere and polyimide hybrid for flexible OLEDs.

PubMed

Kim, Min Kyu; Kim, Dong Won; Shin, Dong Wook; Seo, Sang Joon; Chung, Ho Kyoon; Yoo, Ji Beom

2015-01-28

The fabrication of interlayer dielectrics (ILDs) in flexible organic light-emitting diodes (OLEDs) not only requires flexible materials with a low dielectric constant, but also ones that possess the electrical, thermal, chemical, and mechanical properties required for optimal device performance. Porous polymer-silica hybrid materials were prepared to satisfy these requirements. Hollow SiO2 spheres were synthesized using atomic layer deposition (ALD) and a thermal calcination process. The hybrid film, which consists of hollow SiO2 spheres and polyimide, shows a low dielectric constant of 1.98 and excellent thermal stability up to 500 °C. After the bending test for 50 000 cycles, the porous hybrid film exhibits no degradation in its dielectric constant or leakage current. These results indicate that the hybrid film made up of hollow SiO2 spheres and polyimide (PI) is useful as a flexible insulator with a low dielectric constant and high thermal stability for flexible OLEDs.

Release of MEMS devices with hard-baked polyimide sacrificial layer

NASA Astrophysics Data System (ADS)

Boroumand Azad, Javaneh; Rezadad, Imen; Nath, Janardan; Smith, Evan; Peale, Robert E.

2013-03-01

Removal of polyimides used as sacrificial layer in fabricating MEMS devices can be challenging after hardbaking, which may easily result by the end of multiple-step processing. We consider the specific commercial co-developable polyimide ProLift 100 (Brewer Science). Excessive heat hardens this material, so that during wet release in TMAH based solvents, intact sheets break free from the substrate, move around in the solution, and break delicate structures. On the other hand, dry reactive-ion etching of hard-baked ProLift is so slow, that MEMS structures are damaged from undesirably-prolonged physical bombardment by plasma ions. We found that blanket exposure to ultraviolet light allows rapid dry etch of the ProLift surrounding the desired structures without damaging them. Subsequent removal of ProLift from under the devices can then be safely performed using wet or dry etch. We demonstrate the approach on PECVD-grown silicon-oxide cantilevers of 100 micron × 100 micron area supported 2 microns above the substrate by ~100-micron-long 8-micron-wide oxide arms.

The Wettability of LaRC Colorless Polyimide Resins on Casting Surfaces

NASA Technical Reports Server (NTRS)

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

1997-01-01

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

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).

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.

Determining resin/fiber content of laminates

NASA Technical Reports Server (NTRS)

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

1979-01-01

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

Repair techniques for celion/LARC-160 graphite/polyimide composite structures

NASA Technical Reports Server (NTRS)

Jones, J. S.; Graves, S. R.

1984-01-01

The large stiffness-to-weight and strength-to-weight ratios of graphite composite in combination with the 600 F structural capability of the polyimide matrix can reduce the total structure/TPS weight of reusable space vehicles by 20-30 percent. It is inevitable that with planned usage of GR/PI structural components, damage will occur either in the form of intrinsic flaw growth or mechanical damage. Research and development programs were initiated to develop repair processes and techniques specific to Celion/LARC-160 GR/PI structure with emphasis on highly loaded and lightly loaded compression critical structures for factory type repair. Repair processes include cocure and secondary bonding techniques applied under vacuum plus positive autoclave pressure. Viable repair designs and processes are discussed for flat laminates, honeycomb sandwich panels, and hat-stiffened skin-stringer panels. The repair methodology was verified through structural element compression tests at room temperature and 315 C (600 F).

Comparative study of all-printed polyimide humidity sensors with single- and multiwalled carbon nanotube gas-permeable top electrodes

NASA Astrophysics Data System (ADS)

Itoh, Eiji; Yuan, Zihan

2017-05-01

We have developed printed capacitive humidity sensors with highly gas permeable carbon nanotube top electrodes using solution techniques. The hydrophobic, porous multiwalled carbon nanotube (MWCNT) network was suitable for gas permeation, and the response of the capacitive humidity sensors was faster than that of a device with a single-walled carbon nanotube (SWCNT) top electrode. The newly developed measurement system consisting of a small measurement chamber, a computer-controlled high-speed solenoid valve, and a mass-flow controller enabled us to vary the ambient relative humidity within 0.1 s. A comparative study of the devices consisting of a 1.1-µm-thick partially fluorinated polyimide dielectric layer and an MWCNT or SWCNT top electrode revealed that the rise time (humidification process) of the device with MWCNTs (0.49 s) in the transient measurement was almost 3 times shorter than that with SWCNTs (1.48 s) owing to the hydrophobic surface of the MWCNTs. A much larger difference was observed during the drying process (recovery time) probably owing to the hydrophilic parts of the SWCNT surface. It was revealed that the response time was almost proportional to the square of the thickness of the polyimide dielectric layer, d, and the sensitivity was inversely proportional to d. The rise time decreased to 0.15 s and a sensitivity per unit area of 12.1 pF %RH-1 cm-2 was obtained in a device with 0.6-µm-thick polyimide and MWCNT top electrodes. This value is suitable for use in high-speed humidity sensors to realize a real-time humidity and breath-sensing measurement system.

Manufacturing Large Membrane Mirrors at Low Cost

NASA Technical Reports Server (NTRS)

2007-01-01

Relatively inexpensive processes have been developed for manufacturing lightweight, wide-aperture mirrors that consist mainly of reflectively coated, edge-supported polyimide membranes. The polyimide and other materials in these mirrors can withstand the environment of outer space, and the mirrors have other characteristics that make them attractive for use on Earth as well as in outer space: With respect to the smoothness of their surfaces and the accuracy with which they retain their shapes, these mirrors approach the optical quality of heavier, more expensive conventional mirrors. Unlike conventional mirrors, these mirrors can be stowed compactly and later deployed to their full sizes. In typical cases, deployment would be effected by inflation. Potential terrestrial and outer-space applications for these mirrors include large astronomical telescopes, solar concentrators for generating electric power and thermal power, and microwave reflectors for communication, radar, and short-distance transmission of electric power. The relatively low cost of manufacturing these mirrors stems, in part, from the use of inexpensive tooling. Unlike in the manufacture of conventional mirrors, there is no need for mandrels or molds that have highly precise surface figures and highly polished surfaces. The surface smoothness is an inherent property of a polyimide film. The shaped area of the film is never placed in contact with a mold or mandrel surface: Instead the shape of a mirror is determined by a combination of (1) the shape of a fixture that holds the film around its edge and (2) control of manufacturing- process parameters. In a demonstration of this manufacturing concept, spherical mirrors having aperture diameters of 0.5 and 1.0 m were fabricated from polyimide films having thicknesses ranging from <20 m to 150 m. These mirrors have been found to maintain their preformed shapes following deployment.

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.

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.

LABCOM resonator Phase 3

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

Keres, L.J.

1990-11-01

The purpose of this project was to develop quartz crystal resonator designs, production processes, and test capabilities for 5-MHz, 6.2-MHz, and 10-MHz resonators for Tactical Miniature Crystal Oscillator (TMXO) applications. GE Neutron Devices (GEND) established and demonstrated the capability to produce and test quartz crystal resonators for use in the TMXO developed by the US Army ERADCOM (now LABCOM). The goals in this project were based on the ERADCOM statement of work. The scope of work indicated that the resonator production facilities for this project would not be completely independent, but that they would be supported in part by equipmentmore » and processes in place at GEND used in US Department of Energy (DOE) work. In addition, provisions for production test equipment or or eventual technology transfer costs to a commercial supplier were clearly excluded from the scope of work. The demonstrated technical capability of the deep-etched blank design is feasible and practical. It can be manufactured in quantity with reasonable yield, and its performance is readily predictable. The ceramic flatpack is a very strong package with excellent hermeticity. The four-point mount supports the crystal to reasonable shock levels and does not perturb the resonator's natural frequency-temperature behavior. The package can be sealed with excellent yields. The high-temperature, high-vacuum processing developed for the TMXO resonator, including bonding the piezoid to its mount with conductive polyimide adhesive, is consistent with precision resonator fabrication. 1 fig., 6 tabs.« less

Structural Evolution and Mechanical Properties of PMR-15/Layered Silicate Nanocomposites

NASA Technical Reports Server (NTRS)

Campbell, Sandi (Technical Monitor); Dean, Derrick; Abdalla, Mohamed; Green, Keith; Small, Sharee

2003-01-01

In the first year of this research, we successfully synthesized and characterized Polymer/ Layered Silicate nanocomposite using the polyimide PMR-15 as the polymer and several layered silicate nanoparticles. We have scaled up the process to allow fabrication of monoliths using these nanocomposites. The morphology of these systems was found to evolve during processing to an exfoliated structure for one system and intercalated for the rest. Correlation with Transmission Electron Microscopy studies is underway. Dynamic mechanical analysis (DMA) results showed a significant increase in the thermomechanical properties (E' and E'') of 2.5 wt.% clay loaded nanocomposites in comparison to the neat polyimide. Increasing the clay loading to 5 wt.% decreased these properties. Higher glass transition temperatures were observed for 2.5 wt.% nanocomposites compared to the neat polyimide. A lower coefficient of thermal expansion was observed only for the PGV/PMR-15 nanocomposite. An improvement in the flexural properties (modulus, strength and elongation) was observed for the 2.5 wt.% nanocomposite but not for the 5 wt.% nanocomposites. The improved barrier properties polymer/ silicate nanocomposites suggest that moisture uptake should be decreased for PMR-15 nanocomposites. The results of some recent experiments to examine delineate the ability of the silicate nanoparticles in improving the hydrolytic degradation of PMR-15 will be discussed.

Dry transfer of graphene to dielectrics and flexible substrates using polyimide as a transparent and stable intermediate layer

NASA Astrophysics Data System (ADS)

Marchena, Miriam; Wagner, Frederic; Arliguie, Therese; Zhu, Bin; Johnson, Benedict; Fernández, Manuel; Lai Chen, Tong; Chang, Theresa; Lee, Robert; Pruneri, Valerio; Mazumder, Prantik

2018-07-01

We demonstrate the direct transfer of graphene from Cu foil to rigid and flexible substrates, such as glass and PET, using as an intermediate layer a thin film of polyimide (PI) mixed with an aminosilane (3-aminopropyltrimethoxysilane) or only PI, respectively. While the dry removal of graphene by an adhesive has been previously demonstrated—being removed from graphite by scotch tape or from a Cu foil by thick epoxy (~20 µm) on Si—our work is the first step towards making a substrate ready for device fabrication using the polymer-free technique. Our approach leads to an article that is transparent, thermally stable—up to 350 °C—and free of polymer residues on the device side of the graphene, which is contrary to the case of the standard wet-transfer process using PMMA. Also, in addition to previous novelty, our technique is fast and easier by using current industrial technology—a hot press and a laminator—with Cu recycling by its mechanical peel-off; it provides high interfacial stability in aqueous media and it is not restricted to a specific material—polyimide and polyamic acids can be used. All the previous reasons demonstrate a feasible process that enables device fabrication.

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.

Irreversible bonding of polyimide and polydimethylsiloxane (PDMS) based on a thiol-epoxy click reaction

NASA Astrophysics Data System (ADS)

Hoang, Michelle V.; Chung, Hyun-Joong; Elias, Anastasia L.

2016-10-01

Polyimide is one of the most popular substrate materials for the microfabrication of flexible electronics, while polydimethylsiloxane (PDMS) is the most widely used stretchable substrate/encapsulant material. These two polymers are essential in fabricating devices for microfluidics, bioelectronics, and the internet of things; bonding these materials together is a crucial challenge. In this work, we employ click chemistry at room temperature to irreversibly bond polyimide and PDMS through thiol-epoxy bonds using two different methods. In the first method, we functionalize the surfaces of the PDMS and polyimide substrates with mercaptosilanes and epoxysilanes, respectively, for the formation of a thiol-epoxy bond in the click reaction. In the second method, we functionalize one or both surfaces with mercaptosilane and introduce an epoxy adhesive layer between the two surfaces. When the surfaces are bonded using the epoxy adhesive without any surface functionalization, an extremely small peel strength (<0.01 N mm-1) is measured with a peel test, and adhesive failure occurs at the PDMS surface. With surface functionalization, however, remarkably higher peel strengths of ~0.2 N mm-1 (method 1) and  >0.3 N mm-1 (method 2) are observed, and failure occurs by tearing of the PDMS layer. We envision that the novel processing route employing click chemistry can be utilized in various cases of stretchable and flexible device fabrication.

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.

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.

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.

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

NASA Technical Reports Server (NTRS)

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

1991-01-01

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

An improved processible acetylene-terminated polyimide for composites

NASA Technical Reports Server (NTRS)

Landis, A. L.; Naselow, A. B.

1985-01-01

The newest member of a family of thermosetting acetylene-substituted polyimide oligomers is HR600P. This oligomer is the isoimide version of the oligomer known as HR600P and Thermid 600. Although both types of material yield the same heat resistant end products after cure, HR600P has much superior processing characteristics. This attributed to its lower melting temperature (160 + or - 10 C, 320 + or - 20 F) in contrast to 202 C (396 F) for Thermid MC-600, its longer gel time at its processing temperature (16 to 30 minutes bvs 3 minutes), and its excellent solubility in low boiling solvents such as tetrahydrofuran, glymes, or 4:1 methyl ethyl ketone/toluene mixtures. These advantages provide more acceptable coating and impregnation procedures, allow for more complete removal at lower temperatures, provide a longer pot life or working time, and allow composite structure fabrication in conventional autoclaves used for epoxy composite curing. The excellent processing characteristics of HR600P allow its use in large area laminated structures, structural composites, and molding compositions.

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.

Small feature sizes and high aperture ratio organic light-emitting diodes by using laser-patterned polyimide shadow masks

NASA Astrophysics Data System (ADS)

Kajiyama, Yoshitaka; Joseph, Kevin; Kajiyama, Koichi; Kudo, Shuji; Aziz, Hany

2014-02-01

A shadow mask technique capable of realizing high resolution (>330 pixel-per-inch) and ˜100% aperture ratio Organic Light-Emitting Diode (OLED) full color displays is demonstrated. The technique utilizes polyimide contact shadow masks, patterned by laser ablation. Red, green, and blue OLEDs with very small feature sizes (<25 μm) are fabricated side by side on one substrate. OLEDs fabricated via this technique have the same performance as those made by established technology. This technique has a strong potential to achieve high resolution OLED displays via standard vacuum deposition processes even on flexible substrates.

Rod-Coil Block Polyimide Copolymers

NASA Technical Reports Server (NTRS)

Meador, Mary Ann B. (Inventor); Kinder, James D. (Inventor)

2005-01-01

This invention is a series of rod-coil block polyimide copolymers that are easy to fabricate into mechanically resilient films with acceptable ionic or protonic conductivity at a variety of temperatures. The copolymers consist of short-rigid polyimide rod segments alternating with polyether coil segments. The rods and coil segments can be linear, branched or mixtures of linear and branched segments. The highly incompatible rods and coil segments phase separate, providing nanoscale channels for ion conduction. The polyimide segments provide dimensional and mechanical stability and can be functionalized in a number of ways to provide specialized functions for a given application. These rod-coil black polyimide copolymers are particularly useful in the preparation of ion conductive membranes for use in the manufacture of fuel cells and lithium based polymer batteries.

Polyimide/metal composite films via in situ decomposition of inorganic additives - Soluble polyimide versus polyimide precursor

NASA Technical Reports Server (NTRS)

Rancourt, J. D.; Porta, G. M.; Moyer, E. S.; Madeleine, D. G.; Taylor, L. T.

1988-01-01

Polyimide-metal oxide (Co3O4 or CuO) composite films have been prepared via in situ thermal decomposition of cobalt (II) chloride or bis(trifluoroacetylacetonato)copper(II). A soluble polyimide (XU-218) and its corresponding prepolymer (polyamide acid) were individually employed as the reaction matrix. The resulting composites exhibited a greater metal oxide concentration at the air interface with polyamide acid as the reaction matrix. The water of imidization that is released during the concurrent polyamide acid cure and additive decomposition is believed to promote metal migration and oxide formation. In contrast, XU-218 doped with either HAuCl4.3H2O or AgNO3 yields surface gold or silver when thermolyzed (300 C).

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.

Processable high temperature resistant polymer matrix materials

NASA Technical Reports Server (NTRS)

Serafini, T. T.

1975-01-01

Studies conducted with addition-type polyimides are reviewed with emphasis on the development of the Polymerization of Monomer Reactants (PMR) approach, in which PMR occurs on the surface of the reinforcing fibers.

Substrate Material for Holographic Emulsions Utilizing Fluorinated Polyimide Film

NASA Technical Reports Server (NTRS)

Gierow, Paul A. (Inventor); Clayton, William R. (Inventor); St.Clair, Anne K. (Inventor)

1999-01-01

A new holographic substrate utilizing flexible. optically transparent fluorinated polyimides. Said substrates have 0 extremely low birefringence which results in a high signal to noise ratio in subsequent holograms. Specific examples of said fluorinated polyimides include 6FDA+APB and 6FDA+4BDAF.

Polyimides containing meta-biphenylenedioxy moieties and articles prepared therefrom

NASA Technical Reports Server (NTRS)

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

1995-01-01

Two monomers containing meta-biphenylenedioxy moieties were prepared. One monomer, a diamine, is used to prepare polyimide, polyamide, and epoxy polymers. The other monomer, a dianhydride, was used to prepared polyimide polymers. These polymers are used to make films, coatings, and selective membranes.

The mechanical stability of polyimide films at high pH

NASA Technical Reports Server (NTRS)

Croall, Catharine I.; St.clair, Terry L.

1990-01-01

Polyimide insulated electrical wire has been widely used in the aerospace industry in commercial, military, and to a lesser degree, general aviation aircraft since the early 1970s. Wiring failures linked to insulation damage have drawn much attention in the media and concerns have developed regarding the long term stability and safety of polyimide insulated electrical wire. The mechanical durability and chemical stability of polyimide insulated wire are affected by hydrolysis, notch propagation, wet and dry arc tracking, topcoat flaking, and degradation due to high pH fluids. Several polyimides were selected for evaluation for resistance to degradation by various aqueous alkaline solutions. The polyimides under evaluation include commercially available films such as KAPTON (tradename), APICAL (tradename), LARC-TPI, and UPILEX (tradename) R and S, as well as a number of experimental films prepared at NASA-Langley. Material properties investigated include viscosity, solubility, moisture absorption, glass transition temperature, dielectric constant, and mechanical properties before and after exposure to various conditions.

Low dielectric constant and moisture-resistant polyimide aerogels containing trifluoromethyl pendent groups

NASA Astrophysics Data System (ADS)

Wu, Tingting; Dong, Jie; Gan, Feng; Fang, Yuting; Zhao, Xin; Zhang, Qinghua

2018-05-01

Conventional polyimide aerogels made from biphenyl-3,3‧,4,4‧-tetracarboxylic dianydride (BPDA) and 4,4‧-oxidianiline (ODA) exhibit poor resistance to moisture and mechanical properties. In this work, a versatile diamine, 2,2‧-bis-(trifluoromethyl)-4,4‧-diaminobiphenyl (TFMB), is introduced to BPDA/ODA backbone to modify the comprehensive performance of this aerogel. Among all formulations, the resulted polyimide aerogels exhibit the lowest shrinkage and density as well as highest porosity, at the ODA/TFMB molar ratio of 5/5. Dielectric constants and loss tangents of the aerogels fall in the range of 1.29-1.33 and 0.001-0.004, respectively, and more TFMB fractions results in a slightly decrease of dielectric constant and loss tangent. In addition, moisture-resistance of the aerogels are dramatically enhanced as the water absorption decreasing from 415% for BPDA/ODA to 13% for the polyimide aerogel at the ODA/TFMB molar ratio of 7/3, and even to 4% for the homo-BPDA/TFMB polyimide aerogel, showing a superhydrophobic characteristic, which is a great advantage for polyimide aerogels used as low dielectric materials. Meanwhile, all of formulations of aerogels exhibit high absorption capacities for oils and common organic solvents, indicating that these fluorinated polyimide aerogels are good candidates for the separation of oils/organic solvents and water. Mechanical properties and thermal stability of the polyimide aerogels are also raised to varying degrees due to the rigid-rod biphenyl structure introduced by TFMB.

New rapid-curing, stable polyimide polymers with high-temperature strength and thermal stability

NASA Technical Reports Server (NTRS)

Burns, E. A.; Jones, J. F.; Kendrick, W. R.; Lubowitz, H. R.; Thorpe, R. S.; Wilson, E. R.

1969-01-01

Additive-type polymerization reaction forms thermally stable polyimide polymers, thereby eliminating the volatile matter attendant with the condensation reaction. It is based on the utilization of reactive alicyclic rings positioned on the ends of polyimide prepolymers having relatively low molecular weights.

Synthesis and Characterization of Polyimides with Ether Linkages

NASA Technical Reports Server (NTRS)

Chuang, Kathy C.; Fu, Joyce; Scheiman, Daniel A.

1998-01-01

A series of polyimides derived from a newly synthesized diamine, namely, 4,4-bis(4-aminophenoxy)-2,2-dimethylbiphenyl (BAPD), were developed and characterized. Their physical and thermal properties were compared to polyimides based on'commercially available 2,2-bis(4-(4-aminophenoxy)phenyl)propane (BAPP).

High density circuit technology, part 2

NASA Technical Reports Server (NTRS)

Wade, T. E.

1982-01-01

A multilevel metal interconnection system for very large scale integration (VLSI) systems utilizing polyimides as the interlayer dielectric material is described. A complete characterization of polyimide materials is given as well as experimental methods accomplished using a double level metal test pattern. A low temperature, double exposure polyimide patterning procedure is also presented.

77 FR 62259 - Certain Polyimide Films, Products Containing Same, and Related Methods Commission Determination...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-10-12

... INTERNATIONAL TRADE COMMISSION [Investigation No. 337-TA-772] Certain Polyimide Films, Products... polyimide films, products containing same, and related methods by reason of infringement of one or more of... prong of the domestic industry requirement. Id. With respect to the `961 patent, the Commission...

77 FR 47092 - Certain Polyimide Films, Products Containing Same, and Related Methods; Notice of Commission...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-08-07

... INTERNATIONAL TRADE COMMISSION [Investigation No. 337-TA-772] Certain Polyimide Films, Products Containing Same, and Related Methods; Notice of Commission Determination to Partially Review and Partially... polyimide films, products containing same, and related methods by reason of infringement of one or more of...

Diphenylmethane-containing dianhydride and polyimides prepared therefrom

NASA Technical Reports Server (NTRS)

St.clair, Anne K. (Inventor); Boston, Harold G. (Inventor); Pratt, J. Richard (Inventor)

1993-01-01

A high temperature stable, highly optically transparent-to-colorless, low dielectic linear aromatic polyimide is prepared by reacting an aromatic diamine with 3,3'bis (3,4-dicarboxyphenoxy) diphenylmethane dianhydride in an amide solvent to form a linear aromatic polyamic acid. This polyamic acid is then cyclized to form the corresponding polyimide.

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.

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.

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.

Polyimide based amorphous silicon solar modules

NASA Technical Reports Server (NTRS)

Jeffrey, Frank R.; Grimmer, Derrick P.; Martens, Steven A.; Abudagga, Khaled; Thomas, Michael L.; Noak, Max

1993-01-01

Requirements for space power are increasingly emphasizing lower costs and higher specific powers. This results from new fiscal constraints, higher power requirements for larger applications, and the evolution toward longer distance missions such as a Lunar or Mars base. The polyimide based a-Si modules described are being developed to meet these needs. The modules consist of tandem a-Si solar cell material deposited directly on a roll of polyimide. A laser scribing/printing process subdivides the deposition into discrete cell strips which are series connected to produce the required voltage without cutting the polymer backing. The result is a large, monolithic, blanket type module approximately 30 cm wide and variable in length depending on demand. Current production modules have a specific power slightly over 500 W/Kg with room for significant improvement. Costs for the full blanket modules range from $30/Watt to $150/Watt depending on quantity and engineering requirements. Work to date focused on the modules themselves and adjusting them for the AMO spectrum. Work is needed yet to insure that the modules are suitable for the space environment.

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.

A novel polyimide based micro heater with high temperature uniformity

DOE PAGES

Yu, Shifeng; Wang, Shuyu; Lu, Ming; ...

2017-02-06

MEMS based micro heaters are a key component in micro bio-calorimetry, nondispersive infrared gas sensors, semiconductor gas sensors and microfluidic actuators. A micro heater with a uniform temperature distribution in the heating area and short response time is desirable in ultrasensitive temperature-dependent measurements. In this study, we propose a novel micro heater design to reach a uniform temperature in a large heating area by optimizing the heating power density distribution in the heating area. A polyimide membrane is utilized as the substrate to reduce the thermal mass and heat loss which allows for fast thermal response as well as amore » simplified fabrication process. A gold and titanium heating element is fabricated on the flexible polyimide substrate using the standard MEMS technique. The temperature distribution in the heating area for a certain power input is measured by an IR camera, and is consistent with FEA simulation results. Finally, this design can achieve fast response and uniform temperature distribution, which is quite suitable for the programmable heating such as impulse and step driving.« less

A novel polyimide based micro heater with high temperature uniformity

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

Yu, Shifeng; Wang, Shuyu; Lu, Ming

MEMS based micro heaters are a key component in micro bio-calorimetry, nondispersive infrared gas sensors, semiconductor gas sensors and microfluidic actuators. A micro heater with a uniform temperature distribution in the heating area and short response time is desirable in ultrasensitive temperature-dependent measurements. In this study, we propose a novel micro heater design to reach a uniform temperature in a large heating area by optimizing the heating power density distribution in the heating area. A polyimide membrane is utilized as the substrate to reduce the thermal mass and heat loss which allows for fast thermal response as well as amore » simplified fabrication process. A gold and titanium heating element is fabricated on the flexible polyimide substrate using the standard MEMS technique. The temperature distribution in the heating area for a certain power input is measured by an IR camera, and is consistent with FEA simulation results. Finally, this design can achieve fast response and uniform temperature distribution, which is quite suitable for the programmable heating such as impulse and step driving.« less

Integrated Electrical Wire Insulation Repair System

NASA Technical Reports Server (NTRS)

Williams, Martha; Jolley, Scott; Gibson, Tracy; Parks, Steven

2013-01-01

An integrated system tool will allow a technician to easily and quickly repair damaged high-performance electrical wire insulation in the field. Low-melt polyimides have been developed that can be processed into thin films that work well in the repair of damaged polyimide or fluoropolymer insulated electrical wiring. Such thin films can be used in wire insulation repairs by affixing a film of this low-melt polyimide to the damaged wire, and heating the film to effect melting, flow, and cure of the film. The resulting repair is robust, lightweight, and small in volume. The heating of this repair film is accomplished with the use of a common electrical soldering tool that has been modified with a special head or tip that can accommodate the size of wire being repaired. This repair method can furthermore be simplified for the repair technician by providing replaceable or disposable soldering tool heads that have repair film already "loaded" and ready for use. The soldering tool heating device can also be equipped with a battery power supply that will allow its use in areas where plug-in current is not available

Silicone Coating on Polyimide Sheet

NASA Technical Reports Server (NTRS)

Park, J. J.

1985-01-01

Silicone coatings applied to polyimide sheeting for variety of space-related applications. Coatings intended to protect flexible substrates of solar-cell blankets from degradation by oxygen atoms, electrons, plasmas, and ultraviolet light in low Earth orbit and outer space. Since coatings are flexible, generally useful in forming flexible laminates or protective layers on polyimide-sheet products.

Dimensionally Stable Ether-Containing Polyimide Copolymers

NASA Technical Reports Server (NTRS)

Fay, Catharine C. (Inventor); St.Clair, Anne K. (Inventor)

1999-01-01

Novel polyimide copolymers containing ether linkages were prepared by the reaction of an equimolar amount of dianhydride and a combination of diamines. The polyimide copolymers described herein possess the unique features of low moisture uptake, dimensional stability, good mechanical properties, and moderate glass transition temperatures. These materials have potential application as encapsulants and interlayer dielectrics.

Polyimide Aerogels with Three-Dimensional Cross-Linked Structure

NASA Technical Reports Server (NTRS)

Meador, Mary Ann B. (Inventor)

2016-01-01

A method for creating a three dimensional cross-linked polyimide structure includes dissolving a diamine, a dianhydride, and a triamine in a solvent, imidizing a polyamic acid gel by heating the gel, extracting the gel in a second solvent, supercritically drying the gel, and removing the solvent to create a polyimide aerogel.

Reinforced Thermoplastic Polyimide with Dispersed Functionalized Single Wall Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Lebron-Colon, Marisabel; Meador, Michael A.; Gaier, James R.; Sola, Francisco; Scheiman, Daniel A.; McCorkle, Linda S.

2010-01-01

Molecular pi-complexes were formed from pristine HiPCO single-wall carbon nanotubes (SWCNTs) and 1-pyrene- N-(4- N'-(5-norbornene-2,3-dicarboxyimido)phenyl butanamide, 1. Polyimide films were prepared with these complexes as well as uncomplexed SWCNTs and the effects of nanoadditive addition on mechanical, thermal, and electrical properties of these films were evaluated. Although these properties were enhanced by both nanoadditives, larger increases in tensile strength and thermal and electrical conductivities were obtained when the SWCNT/1 complexes were used. At a loading level of 5.5 wt %, the Tg of the polyimide increased from 169 to 197 C and the storage modulus increased 20-fold (from 142 to 3045 MPa). The addition of 3.5 wt % SWCNT/1 complexes increased the tensile strength of the polyimide from 61.4 to 129 MPa; higher loading levels led to embrittlement and lower tensile strengths. The electrical conductivities (DC surface) of the polyimides increased to 1 x 10(exp -4) Scm(exp -1) (SWCNT/1 complexes loading level of 9 wt %). Details of the preparation of these complexes and their effects on polyimide film properties are discussed.

Fabrication and evaluation of dispersed-Ag nanoparticles-in-polyimide thin films

NASA Astrophysics Data System (ADS)

Sonehara, Makoto; Watanabe, Yuki; Yamaguchi, Sota; Kato, Takanori; Yoshisaku, Yasuaki; Sato, Toshiro; Itoh, Eiji

2017-10-01

A thin-film common-mode filter (TF-CMF) for cell phones in the UHF band was fabricated and evaluated. The TF-CMF consisted of multiple metal-insulator-metal (MIM) capacitors and inductors. The sizes of the 0.70-1.0 GHz band-type and 1.8-2.0 GHz band-type TF-CMFs are 1,140 × 1,260 × 10.5 µm3, and 1,060 × 1,060 × 10.5 µm3, respectively. The footprint in both types of TF-CMFs is over 1 mm2. In order to miniaturize the TF-CMF, we proposed to change a polyimide-only to a polyimide with dispersed Ag nanoparticles with high permittivity in the insulator layer for the MIM capacitor of the TF-CMF. A polyimide (\\text{polyimide precursor}:\\text{toluene with dispersed Ag nanoparticles} = 100:1) thin film with dispersed high-density Ag nanoparticles has a relative permittivity of about 8, which is twice as high as that of the polyimide-only thin film. If the capacitance and distance between electrodes are the same, then the capacitor footprint may be halved.

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.

Polyimide Aerogel Thin Films

NASA Technical Reports Server (NTRS)

Meador, Mary Ann; Guo, Haiquan

2012-01-01

Polyimide aerogels have been crosslinked through multifunctional amines. This invention builds on "Polyimide Aerogels With Three-Dimensional Cross-Linked Structure," and may be considered as a continuation of that invention, which results in a polyimide aerogel with a flexible, formable form. Gels formed from polyamic acid solutions, end-capped with anhydrides, and cross-linked with the multifunctional amines, are chemically imidized and dried using supercritical CO2 extraction to give aerogels having density around 0.1 to 0.3 g/cubic cm. The aerogels are 80 to 95% porous, and have high surface areas (200 to 600 sq m/g) and low thermal conductivity (as low as 14 mW/m-K at room temperature). Notably, the cross-linked polyimide aerogels have higher modulus than polymer-reinforced silica aerogels of similar density, and can be fabricated as both monoliths and thin films.

Advanced Polymers Containing the Phenyltrifluoroethylidene Connecting Group

NASA Technical Reports Server (NTRS)

Alstron, William B.; Sivko, Gloria S.

2006-01-01

A new, lower cost fluorinated dianhydride based on the phenyltrifluoroethylidene (3F) connecting linkage was invented by the principal author in the early 1980's. New 3F condensation and addition cured polyimides were synthesized with the newly discovered 3F dianhydride and the previously known 3F diamine. As controls, polyimides based on the somewhat analogous higher cost hexafluoroisopropylidene (6F) linkage were also prepared. The short term thermal oxidative stability (TOS), determined by thermal gravimetric analysis (TGA), and the glass transition temperatures (Tg) of 3F dianhydride polyimides were found to be similar to 6F dianhydride polyimides, but the Tg was slightly higher for 3F diamine polyimides than 6F diamine polyimides. Unfortunately, in real time testing, long term TOS of 3F polymers was clearly inferior to 6F polymers. This was due to a 3 to 5 fold greater rate of loss of trifluoromethyl group from 3F versus 6F linkages. However, at shorter times or lower temperatures, 3F TOS was almost comparable to 6F TOS. The wide scope of the 3F technology was also demonstrated to have distinct unique advantages over 6F technology through the use of the 3F pendant phenyl ring as a synthetic site to introduce other functional groups. These groups have been used for the control or modification of polymer properties; an advantage lacking within 6F technology. The synthetic ease by which 3F can be introduced into various types of monomers has lead to the explosion of advanced 3F polyimides and other high performance advanced 3F polymers in the prior decade of 3F polymer literature as cited herein; covering polyimides, substituted polyimides, at least ten types of nonpolyimide 3F polymer modifications, and also the government's nine 3F U.S. patents and corporations' nine 3F U.S. patents.

Characterization of cobalt(II) chloride-modified condensation polyimide films

NASA Technical Reports Server (NTRS)

Rancourt, J. D.; Taylor, L. T.

1988-01-01

The effect of solvent extraction on the properties of cobalt(II) chloride-modified polyimide films was investigated. Solvent-cast films were prepared from solutions of cobalt chloride in poly(amide acid)/N,N-dimethylacetamide (DMAc) and were subsequently dried and cured in static air, forced air, or inert gas ovens with controlled humidity. The films were extracted by either of the three processes (1) soaking in a tray with distilled water at room temperature, (2) soxhlett extraction with distilled water, or (3) soxhell extraction with DMAc. Extraction with DMAc was found to remove both cobalt and chlorine from the films and to slightly increase bulk thermal stability and both surface resistivity and electrical resistivity.

Wet spinning of solid polyamic acid fibers

NASA Technical Reports Server (NTRS)

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

1989-01-01

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

Wet spinning of solid polyamic acid fibers

NASA Technical Reports Server (NTRS)

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

1991-01-01

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

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.

Fire-resistant phosphorus containing polyimides and copolyimides

NASA Technical Reports Server (NTRS)

Mikroyannidis, J. A. (Inventor)

1985-01-01

Phosphorus-containing polyimides and copolyimides are synthesized in a two-step polycondensation reaction from 1- (diorganooxyphosphonl)methly 2,4- and 2,6-diaminobenzenes and tetracarboxylic anhydride. The diorgano position of the diorganooxyphosphonyl group includes alkyl, such as ethyl, substituted alkyl, such as 2-chloroethyl, and aryl such as phenyl. The tetracarboxylic anhydries include compounds such as pyrometallitic dianhydride and benzophenone tetracarboxylic dianhydride. The glass transition temperature (Tg) of the polyimides is reduced by incorporation of the (dialkoxyphosphonyl)methyl groups. The phosphorus-containing copolyimides show a considerably higher degree of fire-resistance as compared to that of the corresponding common polyimides.

The hydrolysis of polyimides

NASA Technical Reports Server (NTRS)

Hoagland, P. D.; Fox, S. W.

1973-01-01

Thermal polymerization of aspartic acid produces a polysuccinimide (I), a chain of aspartoyl residues. An investigation was made of the alkaline hydrolysis of the imide rings of (I) which converts the polyimide to a polypeptide. The alkaline hydrolysis of polyimides can be expected to be kinetically complex due to increasing negative charge generated by carboxylate groups. For this reason, a diimide, phthaloyl-DL-aspartoyl-beta-alanine (IIA) was synthesized for a progressive study of the hydrolysis of polyimides. In addition, this diimide (IIA) can be related to thalidomide and might be expected to exhibit similar reactivity during hydrolysis of the phthalimide ring.

Polyimides containing pendent trifluoromethyl groups

NASA Technical Reports Server (NTRS)

Havens, S. J.; Hergenrother, P. M.

1993-01-01

Several new polyimides containing trifluoromethyl groups were prepared from the reaction of various aromatic dianhydrides and two new diamines containing trifluoromethyl groups, 4,4'-bis(3-amino-5-trifluoromethylphenoxy)biphenyl and l,4-bis(3-amino-5-trifluoromethylphenoxy)benzene. The diamines were prepared from the aromatic nucleophilic displacement of the disodium salts of 4,4'-biphenol or hydroquinone with 3,5-dinitrobenzotrifluoride followed by hydrogenation of the resultant dinitro compounds. The thermally cured polyimides exhibited glass transition temperatures between 186 and 262 C. By thermogravimetric analysis, the polyimides exhibited 5 percent weight losses at 484-527 C in nitrogen and 452-506 C in air.

Polyimides: Tribological properties and their use as lubricants

NASA Technical Reports Server (NTRS)

Fusaro, R. L.

1982-01-01

Friction, wear, and wear mechanisms of several different polyimide films, solid bodies, composites, and bonded solid lubricant films are compared and discussed. In addition, the effect of such parameters as temperatures, type of atmosphere, contact stress, and specimen configuration are investigated. A friction and wear transition occurs in some polyimides at elevated temperatures and this transition is related to molecular relaxations that occur in polyimides. Friction and wear data from an accelerated test (pin-on-disk) are compared to similar data from an end use test device (plain spherical bearing), and to other polymers investigated in a similar geometry.

Screening of high temperature adhesives for large area bonding

NASA Technical Reports Server (NTRS)

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

1980-01-01

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

Solution processed flexible organic thin film back-gated transistors based on polyimide dielectric films

NASA Astrophysics Data System (ADS)

Park, Janghoon; Min, Yoonki; Lee, Dongjin

2018-04-01

An organic thin film back-gated transistor (OBGT) was fabricated and characterized. The gate electrode was printed on the back side of substrate, and the dielectric layer was omitted by substituting the dielectric layer with the polyimide (PI) film substrate. Roll-to-roll (R2R) gravure printing, doctor blading, and drop casting methods were used to fabricate the OBGT. The printed OBGT device shows better performance compared with an OTFT device based on dielectric layer of BaTiO3. Additionally, a calendering process enhanced the performance by a factor of 3 to 7 (mobility: 0.016 cm2/V.s, on/off ratio: 9.17×103). A bending test was conducted to confirm the flexibility and durability of the OBGT device. The results show the fabricated device endures 20000-cyclic motions. The realized OBGT device was successfully fabricated and working, which is meaningful for production engineering from the viewpoint of process development.

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

NASA Technical Reports Server (NTRS)

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

2003-01-01

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

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

NASA Technical Reports Server (NTRS)

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

2006-01-01

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

Microwave sintering of Ag-nanoparticle thin films on a polyimide substrate

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

Fujii, S., E-mail: fujii.s.ap@m.titech.ac.jp; Department of Information and Communication System Engineering, National Institute of Technology, Okinawa College, Nago, Okinawa 905-2192; Kawamura, S.

2015-12-15

Ag-nanoparticle thin films on a polyimide substrate were subjected to microwave sintering by use of a single-mode waveguide applicator. A two-step sintering process was employed. First, at low conductivities of the film, the film sample was placed at the site of the maximum electric field and subjected to microwave irradiation. Second, when the conductivity of the film increased, the film sample was placed at the site of the maximum magnetic field and again subjected to microwave irradiation. The microwave sintering process was completed within 1.5 min, which is significantly lower than the time required for the oven heating process. Themore » resulting conductivity of the film, albeit only 30% of that of the bulk material, was seven times that of a film annealed at the same temperature in a furnace. Scanning electron microscopy images revealed that the nanoparticles underwent both grain necking and grain growth during microwave sintering. In addition, this sintering process was equivalent to the oven heating process performed at a 50 °C higher annealing temperature. An electromagnetic wave simulation and a heat transfer simulation of the microwave sintering process were performed to gain a thorough understanding of the process.« less

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

NASA Technical Reports Server (NTRS)

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

2002-01-01

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

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.

Porous tooling process for manufacture of graphite/polyimide composites

NASA Technical Reports Server (NTRS)

Smiser, L. W.; Orr, K. K.; Araujo, S. M.

1981-01-01

A porous tooling system was selected for the processing of Graphite/PMR-15 Polyimide laminates in thickness up to 3.2 mm. (0.125 inch). This tool system must have a reasonable strength, permeability dimensional stability, and thermal conductivity to accomplish curing at 600 F and 200 psi and 200 psi autoclave temperature and pressure. A permeability measuring apparatus was constructed and permeability vs. casting water level determined to produce tools at three different permeability levels. On these tools, laminates of 5, 11, and 22 plies (.027, .060, and 0.121 inch) were produced and evaluated by ultrasonic, mechanical, and thermal tests to determine the effect of the tool permeability on the cured laminates. All tools produced acceptable laminates at 5 and 11 plies but only the highest permeability produced acceptable clear ultrasonic C-Scans. Recommendations are made for future investigations of design geometry, and strengthening techniques for porous ceramic tooling.

Biaxial extrusion of polyimide LARC-TPI and LARC-TPI blends

NASA Technical Reports Server (NTRS)

Haghighat, R. Ross; Elandjian, Lucy; Lusignea, Richard W.

1990-01-01

Biaxial films of polyimide LARC-TPI and LARC-TPI/liquid crystal polymer Xydar were extruded directly from the melt for the first time via an innovative extrusion technique. Three types of films, neat LARC-TPI, LARC-TPI/10 wt pct and 30 wt pct blends were processed as a part of this NASA-funded program. Processability was greatly enhanced by incorporating Xydar. The coefficient of thermal expansion was reduced from 34 ppm/C for the neat LARC-TPI to 15 ppm/C for the 10 wt pct Xydar blend and ultimately down to 1 to 3 ppm/C for the 30 wt pct blend films in the direction of extrusion. The maximum improvement in stiffness was realized by incorporating 10 wt pct Xydar (2.8 GPa up to 4.9 GPa). Tensile strength, however, experienced a drop as a result of Xydar addition, probably caused by inefficient mixing of the two phases.

Conversion of Langmuir-Blodgett monolayers and bilayers of poly(amic acid) through polyimide to graphene

NASA Astrophysics Data System (ADS)

Jo, Hye Jin; Lyu, Ji Hong; Ruoff, Rodney S.; Lim, Hyunseob; In Yoon, Seong; Jeong, Hu Young; Shin, Tae Joo; Bielawski, Christopher W.; Shin, Hyeon Suk

2017-03-01

Various solid carbon sources, particularly poly(methyl methacrylate), have been used as precursors to graphene. The corresponding growth process generally involves the decomposition of the solids to hydrocarbon gases followed by their adsorption on metallic substrates (e.g., Cu). We report a different approach that uses a thermally-resistant polyimide (PI) as a carbon precursor. Langmuir-Blodgett films of poly(amic acid) (PAA) were transferred to copper foils and then converted to graphene via a PI intermediate. The Cu foil substrate was also discovered to facilitate the orientation of aromatic moieties upon carbonization process of the PI. As approximately 50% of the initial quantity of the PAA was found to remain at 1000 °C, thermally-stable polymers may reduce the quantity of starting material required to prepare high quality films of graphene. Graphene grown using this method featured a relatively large domain size and an absence of adventitious adlayers.

Use of laser drilling in the manufacture of organic inverter circuits.

PubMed

Iba, Shingo; Kato, Yusaku; Sekitani, Tsuyoshi; Kawaguchi, Hiroshi; Sakurai, Takayasu; Someya, Takao

2006-01-01

Inverter circuits have been made by connecting two high-quality pentacene field-effect transistors. A uniform and pinhole-free 900 nm thick polyimide gate-insulating layer was formed on a flexible polyimide film with gold gate electrodes and partially removed by using a CO2 laser drilling machine to make via holes and contact holes. Subsequent evaporation of the gold layer results in good electrical connection with a gold gate layer underneath the gate-insulating layer. By optimization of the settings of the CO2 laser drilling machine, contact resistance can be reduced to as low as 3 ohms for 180 microm square electrodes. No degradation of the transport properties of the organic transistors was observed after the laser-drilling process. This study demonstrates the feasibility of using the laser drilling process for implementation of organic transistors in integrated circuits on flexible polymer films.

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.

Tribological properties and thermal stability of various types of polyimide films

NASA Technical Reports Server (NTRS)

Fusaro, R. L.

1981-01-01

Thermal exposure experiments at 315 and 350 C were conducted on seven different types of polyimide films to determine which was the most thermally stable and adherent. The polyimides were ranked according to the rate at which they lost weight and how well they adhere to the metallic substrate. Friction and wear experiments were conducted at 25 C (room temperature) on films bonded to 440C HT stainless steel. Friction, film wear rates, wear mechanisms, and transfer films of the seven films were investigated and compared. The polyimides were found to fall into two groups as far as friction and wear properties were concerned. Group one had lower friction but an order of magnitude higher film wear rate than did group two. The wear mechanism was predominately adhesive, but the size of the wear particles were larger for group one polyimides.

Tribological properties and thermal stability of various types of polyimide films

NASA Technical Reports Server (NTRS)

Fusaro, R. L.

1981-01-01

Thermal exposure experiments at 315 and 350 C were conducted on seven different types of polyimide films to determine which was the most thermally stable and adherent. The polyimides were ranked according to the rate of which they lost weight and how well they adhered to the metallic substrate. Friction and wear experiments were conducted at 25 C (room temperature) on films bonded to 440C HT stainless steel. Friction, film wear rates, wear mechanisms, and transfer films of the seven films were investigated and compared. The polyimides were found to fall into two groups as far as friction and wear properties were concerned. Group I had lower friction but an order of magnitude higher film wear rate than did group II. The wear mechanism was predominately adhesive, but the size of the wear particles was larger for group I polyimides.

Surface Modification of Polyimide for Improving Adhesion Strength by Inductively Coupled Plasma

NASA Astrophysics Data System (ADS)

Byun, Tae Joon; Kim, Sung Il; Kim, Youn Joon; Choi, Yoon Suk; Choi, In Sik; Setsuhara, Yuichi; Geon Han, Jeon

2009-08-01

This study examined the effect of an inductively coupled plasma (ICP) treatment using an argon and helium gas mixture on the adhesion between polyimide and a copper film. Optical emission spectroscopy (OES) of the ICP revealed the emission intensity of helium and argon at various intensities with the helium mixing ratio. The treated polyimide surface was analyzed using a contact angle analyzer, Atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The contact angle and RMS roughness ranged from 66 to 31° and 2.3 to 4.1 nm, respectively. XPS showed an increase in C-O bonding. The highest peel strength was 0.43 kgf/cm at a 40% of helium mixing ratio, which contained the highest level of activate species. Overall, an ICP treatment of a polyimide surface with a 40% helium gas mixture improves the adhesion strength between copper and polyimide significantly.

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.

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.

Molecular Simulation of Ionic Polyimides and Composites with Ionic Liquids as Gas-Separation Membranes.

PubMed

Abedini, Asghar; Crabtree, Ellis; Bara, Jason E; Turner, C Heath

2017-10-24

Polyimides are at the forefront of advanced membrane materials for CO 2 capture and gas-purification processes. Recently, ionic polyimides (i-PIs) have been reported as a new class of condensation polymers that combine structural components of both ionic liquids (ILs) and polyimides through covalent linkages. In this study, we report CO 2 and CH 4 adsorption and structural analyses of an i-PI and an i-PI + IL composite containing [C 4 mim][Tf 2 N]. The combination of molecular dynamics (MD) and grand canonical Monte Carlo (GCMC) simulations is used to compute the gas solubility and the adsorption performance with respect to the density, fractional free volume (FFV), and surface area of the materials. Our results highlight the polymer relaxation process and its correlation to the gas solubility. In particular, the surface area can provide meaningful guidance with respect to the gas solubility, and it tends to be a more sensitive indicator of the adsorption behavior versus only considering the system density and FFV. For instance, as the polymer continues to relax, the density, FFV, and pore-size distribution remain constant while the surface area can continue to increase, enabling more adsorption. Structural analyses are also conducted to identify the nature of the gas adsorption once the ionic liquid is added to the polymer. The presence of the IL significantly displaces the CO 2 molecules from the ligand nitrogen sites in the neat i-PI to the imidazolium rings in the i-PI + IL composite. However, the CH 4 molecules move from the imidazolium ring sites in the neat i-PI to the ligand nitrogen atoms in the i-PI + IL composite. These molecular details can provide critical information for the experimental design of highly selective i-PI materials as well as provide additional guidance for the interpretation of the simulated adsorption systems.

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

Characterization of a thermally imidized soluble polyimide film

NASA Technical Reports Server (NTRS)

Young, Philip R.; Davis, Judith R. J.; Chang, A. C.; Richardson, John N.

1989-01-01

A soluble aromatic poly(amic acid) film was converted to a soluble polyimide by staging at 25 deg intervals to 325 C and characterized at each interval by several analytical methods. The behavior observed was consistent with an interpretation that a reduction occurred in molecular weight of the poly(amic acid) during the initial stages of cure before the ultimate molecular weight was achieved as a polyimide. This interpretation was supported by the results of solution viscosity, gel permeation chromatography, low angle laser light scattering photometry and infrared spectroscopy analysis. The results serve to increase the fundamental understanding of how polyimides are thermally formed from poly(amic acids).

The mechanical properties of polyimide films after exposure to high pH

NASA Technical Reports Server (NTRS)

Croall, Catharine I.; St.clair, Terry L.

1992-01-01

Wiring failures linked to insulation damage have drawn much attention in the aerospace industry and concerns have developed regarding the stability and safety of polyimide insulated electrical wire. Several polyimides were selected for evaluation for resistance to degradation by various aqueous alkaline solutions. The polyimides under evaluation include commercially available films such as Kapton (tk), Apical (tk), LaRC(tk)-TPI, and Upilex(tk)R and S, as well as a number of experimental films prepared by NASA Langley. Thermally imidized films were studied for their retention of mechanical properties after exposure to high pH solutions under stressed conditions.

Effect of using polyimide capillaries during thermal experiments on the particle size distribution of supported Pt nanoparticles

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

Gámez-Mendoza, Liliana; Resto, Oscar; Martínez-Iñesta, María

2015-09-20

Kapton HN-type polyimide capillaries are commonly used as sample holders for transmission X-ray experiments at temperatures below 673 K because of their thermal stability, high X-ray transmittance and low cost. Using high-angle annular dark field scanning high-resolution transmission electron microscopy and thermogravimetric analysis, this work shows that using polyimide capillaries leads to the overgrowth of supported Pt nanoparticles during reduction at temperatures below the glass transition temperature (T g= 658 K) owing to an outgassing of water from the polyimide. Quartz capillaries were also studied and this overgrowth was not observed.

Propagation Characteristics of Finite Ground Coplanar Waveguide on Si Substrates With Porous Si and Polyimide Interface Layers

NASA Technical Reports Server (NTRS)

Ponchak, George E.; Itotia, Isaac K.; Drayton, Rhonda Franklin

2003-01-01

Measured and modeled propagation characteristics of Finite Ground Coplanar (FGC) waveguide fabricated on a 15 ohm-cm Si substrate with a 23 micron thick, 68% porous Si layer and a 20 micron thick polyimide interface layer are presented for the first time. Attenuation and effective permittivity as function of the FGC geometry and the bias between the center conductor and the ground planes are presented. It is shown that the porous Si reduces the attenuation by 1 dB/cm compared to FGC lines with only polyimide interface layers, and the polyimide on porous silicon demonstrates negligible bias dependence.

Highly optical transparency and thermally stable polyimides containing pyridine and phenyl pendant.

PubMed

Yao, Jianan; Wang, Chunbo; Tian, Chengshuo; Zhao, Xiaogang; Zhou, Hongwei; Wang, Daming; Chen, Chunhai

2017-01-01

In order to obtain highly optical transparency polyimides, two novel aromatic diamine monomers containing pyridine and kinky structures, 1,1-bis[4-(5-amino-2-pyridinoxy)phenyl]diphenylmethane (BAPDBP) and 1,1-bis[4-(5-amino-2-pyridinoxy)phenyl]-1-phenylethane (BAPDAP), were designed and synthesized. Polyimides based on BAPDBP, BAPDAP, 2,2-bis[4-(5-amino-2-pyridinoxy)phenyl]propane (BAPDP) with various commercial dianhydrides were prepared for comparison and structure-property relationships study. The structures of the polyimides were characterized by Fourier transform infrared (FT-IR) spectrometer, wide-angle X-ray diffractograms (XRD) and elemental analysis. Film properties including solubility, optical transparency, water uptake, thermal and mechanical properties were also evaluated. The introduction of pyridine and kinky structure into the backbones that polyimides presented good optical properties with 91-97% transparent at 500 nm and a low cut-off wavelength at 353-398 nm. Moreover, phenyl pendant groups of the polyimides showed high glass transition temperatures ( T g ) in the range of 257-281 °C. These results suggest that the incorporating pyridine, kinky and bulky substituents to polymer backbone can improve the optical transparency effectively without sacrificing the thermal properties.

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.

Polyhedral oligomeric silsesquioxane (POSS) polyimides as space-survivable materials

NASA Astrophysics Data System (ADS)

Tomczak, Sandra J.; Vij, Vandana; Marchant, Darrell; Minton, Timothy K.; Brunsvold, Amy L.; Wright, Michael E.; Petteys, Brian J.; Guenthner, Andrew J.; Yandek, Gregory R.; Mabry, Joe

2006-09-01

Polyimides (PIs) such as Kapton are used extensively in spacecraft thermal blankets, solar arrays, and space inflatable structures. Atomic oxygen (AO) in low Earth orbit (LEO) causes severe degradation of Kapton. SiO2 coatings impart remarkable oxidation resistance and have been widely used to protect Kapton, yet imperfections in the SiO2 application process and micrometeoroid/debris impact in orbit damage the SiO2 coating leading to Kapton erosion. A polyimide that is self-passivating by the formation of a silica layer upon exposure to AO has been achieved by the copolymerization of a polyhedral oligomeric silsesquioxane (POSS) diamine with the Kapton monomers, pyromellitic dianhydride and 4,4'-oxydianiline, resulting in POSS-Kapton-polyimide. The self-passivating properties have been shown by monitoring a 1 micron deep scratch in POSS-PIs after exposure to AO. Kapton H, SiO2-coated Kapton HN, and 8.75 weight % Si8O11 cage "main-chain" POSS-polyimide (8.75 wt % Si8O11 MC-POSS-PI) were exposed to equivalent AO fluences before and after being scratched. During the first AO exposure and outside of the scratch, these samples eroded 5.0 microns, 0 microns, and less than 200 nm respectively. During the second AO exposure, the samples eroded an additional 5.0 microns within the scratch and outside of the scratch, 7.0 microns within the scratch and 0 microns outside of the scratch, and 200 nm within the scratch and 0 microns outside of the scratch respectively. Surface analysis of MC-POSS-PI films exposed to a hyperthermal O-atom beam shows evidence for the formation of a SiO2 passivation layer upon AO exposure. This is exemplified by erosion yields of 3.5 and 7 wt % Si8O11 MC-POSS-PI samples which were 3.7 and 0.98 percent, respectively, of the erosion yield for Kapton H at a fluence of 8.5 x 1020 O atoms cm-2. Comparison of MC-POSS-PIs and "side-chain" POSS-PI (SC-POSS-PI) shows that these polymers have similar resistance to atomic oxygen and physical properties similar to Kapton H. Erosion yields and imaging of POSS-PIs flown on MISSE1, in a sample tray exposed to all elements (AO, UV light) of the space environment, demonstrated the greatly extended lifetime of POSS-PIs over polyimide.

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.

Polyimide molding powder, coating, adhesive, and matrix resin

NASA Technical Reports Server (NTRS)

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

1992-01-01

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

A novel addition polyimide adhesive

NASA Technical Reports Server (NTRS)

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

1981-01-01

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

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.

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.

Method to Prepare Processable Polymides with 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 reactive endcapper. The reactive endcappers studied include but should not be limited to 4-phenylethynyl phthalic anhydride (PEPA ), 3-aminophenoxy- 4'-phenylethynylbenzophenone (3-APEB), maleic anhydride (MA) and nadic anhydride (5-norbomene-2,3-dicarboxylic anhydride, NA). 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. By simply changing the ratio of APB to the other diamine in the polyimide backbone, a material with a unique combination of solubility, Tg, Tm, melt viscosity, toughness and elevated temperature mechanical properties can be prepared. The copolymers that result from using APB to enhance processability have a unique combination of properties that include low pressure processing (200 psi and below), long term melt stability (several hours at 300 C. for the phenylethynyl terminated polymers), high toughness, improved solvent resistance, improved adhesive properties, and improved composite mechanical properties. These copolyimides are eminently suitable as adhesives, composite matrices, moldings, films and coatings.

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

NASA Technical Reports Server (NTRS)

Chuang, Kathy

2004-01-01

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

Fabrication of a high-density nano-porous structure on polyimide by using ultraviolet laser irradiation

NASA Astrophysics Data System (ADS)

Ma, Yong-Won; Jeong, Myung Yung; Lee, Sang-Mae; Shin, Bo Sung

2016-03-01

A new approach for fabricating a high-density nano-porous structure on polyimide (PI) by using a 355-nm UV laser is presented here. When PI was irradiated by using a laser, debris that had electrical conductivity was generated. Accordingly, that debris caused electrical defects in the field of electronics. Thus, many researchers have tried to focus on a clean processing without debris. However, this study focused on forming a high density of debris so as to fabricate a nano-porous structure consisting of nanofibers on the PI film. A PI film with closed pores and open pores was successfully formed by using a chemical blowing agent (azodicarbonamide, CBA) in an oven. Samples were precured at 130 °C and cured at 205 °C in sequence so that the closed pores might not coalesce in the film. When the laser irradiated the PI film with closed pores, nanofibers were generated because polyimide was not completely decomposed by photochemical ablation. Our results indicated that a film with micro-closed pores, in conjunction with a 355-nm pulsed laser, can facilitate the fabrication of a high-density nano-porous structure.

Polyimide-Based Capacitive Humidity Sensor

PubMed Central

Steinmaßl, Matthias; Endres, Hanns-Erik; Drost, Andreas; Eisele, Ignaz; Kutter, Christoph; Müller-Buschbaum, Peter

2018-01-01

The development of humidity sensors with simple transduction principles attracts considerable interest by both scientific researchers and industrial companies. Capacitive humidity sensors, based on polyimide sensing material with different thickness and surface morphologies, are prepared. The surface morphology of the sensing layer is varied from flat to rough and then to nanostructure called nanograss by using an oxygen plasma etch process. The relative humidity (RH) sensor selectively responds to the presence of water vapor by a capacitance change. The interaction between polyimide and water molecules is studied by FTIR spectroscopy. The complete characterization of the prepared capacitive humidity sensor performance is realized using a gas mixing setup and an evaluation kit. A linear correlation is found between the measured capacitance and the RH level in the range of 5 to 85%. The morphology of the humidity sensing layer is revealed as an important parameter influencing the sensor performance. It is proved that a nanograss-like structure is the most effective for detecting RH, due to its rapid response and recovery times, which are comparable to or even better than the ones of commercial polymer-based sensors. This work demonstrates the readiness of the developed RH sensor technology for industrialization. PMID:29751632

Graphene as transmissive electrodes and aligning layers for liquid-crystal-based electro-optic devices.

PubMed

Basu, Rajratan; Shalov, Samuel A

2017-07-01

In a conventional liquid crystal (LC) cell, polyimide layers are used to align the LC homogeneously in the cell, and transmissive indium tin oxide (ITO) electrodes are used to apply the electric field to reorient the LC along the field. It is experimentally presented here that monolayer graphene films on the two glass substrates can function concurrently as the LC aligning layers and the transparent electrodes to fabricate an LC cell, without using the conventional polyimide and ITO substrates. This replacement can effectively decrease the thickness of all the alignment layers and electrodes from about 100 nm to less than 1 nm. The interaction between LC and graphene through π-π electron stacking imposes a planar alignment on the LC in the graphene-based cell-which is verified using a crossed polarized microscope. The graphene-based LC cell exhibits an excellent nematic director reorientation process from planar to homeotropic configuration through the application of an electric field-which is probed by dielectric and electro-optic measurements. Finally, it is shown that the electro-optic switching is significantly faster in the graphene-based LC cell than in a conventional ITO-polyimide LC cell.

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.

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

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).

Porous Cross-Linked Polyimide Networks

NASA Technical Reports Server (NTRS)

Meador, Mary Ann B. (Inventor); Guo, Haiquan (Inventor)

2015-01-01

Porous cross-linked polyimide networks are provided. The networks comprise an anhydride end-capped polyamic acid oligomer. The oligomer (i) comprises a repeating unit of a dianhydride and a diamine and terminal anhydride groups, (ii) has an average degree of polymerization of 10 to 50, (iii) 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, and (iv) has been chemically imidized to yield the porous cross-linked polyimide network. Also provided are porous cross-linked polyimide aerogels comprising a cross-linked and imidized anhydride end-capped polyamic acid oligomer, wherein the oligomer comprises a repeating unit of a dianhydride and a diamine, and the aerogel has a density of 0.10 to 0.333 g/cm.sup.3 and a Young's modulus of 1.7 to 102 MPa. Also provided are thin films comprising aerogels, and methods of making porous cross-linked polyimide networks.

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.

Spectroscopic investigation of different concentrations of the vapour deposited copper phthalocyanine as a "guest" in polyimide matrix.

PubMed

Georgiev, Anton; Yordanov, Dancho; Dimov, Dean; Assa, Jacob; Spassova, Erinche; Danev, Gencho

2015-04-05

Nanocomposite layers 250 nm copper phthalocyanine/polyimide prepared by simultaneous vapour deposition of three different sources were studied. Different concentrations of copper phthalocyanine as a "guest" in polyimide matrix as a function of conditions of the preparation have been determined by FTIR (Fourier Transform Infrared) and UV-VIS (Ultraviolet-Visible) spectroscopies. The aim was to estimate the possibility of the spectroscopic methods for quantitative determination of the "guest" and compare with the quality of the polyimide thin films in relation to the "guest" concentration. The band at 1334 cm(-1) has been used for quantitative estimation of "guest" in polyimide matrix. The concentrations of the copper phthalocyanine less than 20% require curve fitting techniques with Fourier self deconvolution. The relationship between "guest" concentrations and degree of imidization, as well as the electronic UV-VIS spectra are discussed in relation to the composition, imidization degree and the two crystallographic modification of the embedded chromophore. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

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.

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.

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.

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).

Impact of pulse thermal processing on the properties of inkjet printed metal and flexible sensors

DOE PAGES

Joshi, Pooran C.; Kuruganti, Teja; Killough, Stephen M.

2015-03-11

In this paper, we report on the low temperature processing of environmental sensors employing pulse thermal processing (PTP) technique to define a path toward flexible sensor technology on plastic, paper, and fabric substrates. Inkjet printing and pulse thermal processing technique were used to realize mask-less, additive integration of low-cost sensors on polymeric substrates with specific focus on temperature, humidity, and strain sensors. The printed metal line performance was evaluated in terms of the electrical conductivity characteristics as a function of post-deposition thermal processing conditions. The PTP processed Ag metal lines exhibited high conductivity with metal sheet resistance values below 100more » mΩ/{whitesquare} using a pulse width as short as 250 μs. The flexible temperature and relative humidity sensors were defined on flexible polyimide substrates by direct printing of Ag metal structures. The printed resistive temperature sensor and capacitive humidity sensor were characterized for their sensitivity with focus on future smart-building applications. Strain gauges were printed on polyimide substrate to determine the mechanical properties of the silver nanoparticle films. Finally, the observed electrical properties of the printed metal lines and the sensitivity of the flexible sensors show promise for the realization of a high performance print-on-demand technology exploiting low thermal-budget PTP technique.« less

Fabrication of a Flexible Amperometric Glucose Sensor Using Additive Processes

PubMed Central

Du, Xiaosong; Durgan, Christopher J.; Matthews, David J.; Motley, Joshua R.; Tan, Xuebin; Pholsena, Kovit; Árnadóttir, Líney; Castle, Jessica R.; Jacobs, Peter G.; Cargill, Robert S.; Ward, W. Kenneth; Conley, John F.; Herman, Gregory S.

2015-01-01

This study details the use of printing and other additive processes to fabricate a novel amperometric glucose sensor. The sensor was fabricated using a Au coated 12.7 μm thick polyimide substrate as a starting material, where micro-contact printing, electrochemical plating, chloridization, electrohydrodynamic jet (e-jet) printing, and spin coating were used to pattern, deposit, chloridize, print, and coat functional materials, respectively. We have found that e-jet printing was effective for the deposition and patterning of glucose oxidase inks with lateral feature sizes between ~5 to 1000 μm in width, and that the glucose oxidase was still active after printing. The thickness of the permselective layer was optimized to obtain a linear response for glucose concentrations up to 32 mM and no response to acetaminophen, a common interfering compound, was observed. The use of such thin polyimide substrates allow wrapping of the sensors around catheters with high radius of curvature ~250 μm, where additive and microfabrication methods may allow significant cost reductions. PMID:26634186

Bulk antimony sulfide with excellent cycle stability as next-generation anode for lithium-ion batteries

PubMed Central

Yu, Denis Y. W.; Hoster, Harry E.; Batabyal, Sudip K.

2014-01-01

Nanomaterials as anode for lithium-ion batteries (LIB) have gained widespread interest in the research community. However, scaling up and processibility are bottlenecks to further commercialization of these materials. Here, we report that bulk antimony sulfide with a size of 10–20 μm exhibits a high capacity and stable cycling of 800 mAh g−1. Mechanical and chemical stabilities of the electrodes are ensured by an optimal electrode-electrolyte system design, with a polyimide-based binder together with fluoroethylene carbonate in the electrolyte. The polyimide binder accommodates the volume expansion during alloying process and fluoroethylene carbonate suppresses the increase in charge transfer resistance of the electrodes. We observed that particle size is not a major factor affecting the charge-discharge capacities, rate capability and stability of the material. Despite the large particle size, bulk antimony sulfide shows excellent rate performance with a capacity of 580 mAh g−1 at a rate of 2000 mA g−1. PMID:24691396

Chemical Fabrication Used to Produce Thin-Film Materials for High Power-to- Weight-Ratio Space Photovoltaic Arrays

NASA Technical Reports Server (NTRS)

Hepp, Aloysius F.; Rybicki, George C.; Raffaelle, Ryne P.; Harris, Jerry D.; Hehemann, David G.; Junek, William; Gorse, Joseph; Thompson, Tracy L.; Hollingsworth, Jennifer A.; Buhro, William E.

2000-01-01

The key to achieving high specific power (watts per kilogram) space solar arrays is the development of a high-efficiency, thin-film solar cell that can be fabricated directly on a flexible, lightweight, space-qualified durable substrate such as Kapton (DuPont) or other polyimide or suitable polymer film. Cell efficiencies approaching 20 percent at AM0 (air mass zero) are required. Current thin-film cell fabrication approaches are limited by either (1) the ultimate efficiency that can be achieved with the device material and structure or (2) the requirement for high-temperature deposition processes that are incompatible with all presently known flexible polyimide or other polymer substrate materials. Cell fabrication processes must be developed that will produce high-efficiency cells at temperatures below 400 degrees Celsius, and preferably below 300 degress Celsius to minimize the problems associated with the difference between the coefficients of thermal expansion of the substrate and thin-film solar cell and/or the decomposition of the substrate.

Quality control developments for graphite/PMR15 polyimide composites materials

NASA Technical Reports Server (NTRS)

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

1979-01-01

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

High density circuit technology, part 4

NASA Technical Reports Server (NTRS)

Wade, T. E.

1982-01-01

An accurate study and evaluation of dielectric thin films is conducted in order to find the material or combination of materials which would optimize NASA'S double layer metal process. Emphasis is placed on polyimide dielectrics because of their reported outstanding dielectric characteristics (including electrical, chemical, thermal, and mechanical) and ease of processing, as well as their rapid acceptance by the semiconductor industry.

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.

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.

Advanced thermoplastic resins, phase 1

NASA Technical Reports Server (NTRS)

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

1991-01-01

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

Characterization of LaRC-CPI semicrystalline polyimide using thermal, dynamic mechanical and dielectric relaxation techniques

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

Rich, D.C.; Huo, P.P.; Liu, C.

1993-12-31

The thermal, dynamic mechanical, and dielectric properties of the semicrystalline thermoplastic polyimide LaRC-CPI were studied. Using differential scanning calorimetry to measure heats of fusion and WAXS to measure crystallinity, the heat of fusion of perfect crystalline LaRC-CPI was determined to be 92 {+-} 2 J/g. DMA and dielectric measurements were performed on three LaRC-CPI films (as received, annealed, and amorphous). Crystallinity was found to reinforce the rubbery state resulting in a higher modulus and broader distribution of relaxation times. Broader relaxation for the crystalline LaRC-CPI was also observed in the dielectric tests. Processing strain and the thermal history were foundmore » to have a significant impact in both dynamic mechanical and dielectric relaxation measurements.« less

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.

Evaluation of Double-Vacuum-Bag Process For Composite Fabrication

NASA Technical Reports Server (NTRS)

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

2004-01-01

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

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.

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.

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.

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.

Structural and Electrical Characteristics of Carbon Nanowalls Synthesized on the Polyimide Film.

PubMed

Kwon, Seok Hun; Kim, Hyung Jin; Choi, Won Seok; Kang, Hyunil

2018-09-01

In this study, the structural and electrical characteristics of carbon nanowalls (CNWs) synthesized on polyimide films were investigated. CNWs were synthesized on polyimide films as various growth times. The cross-section and surface of the CNWs synthesized were examined using FE-SEM. The growth and defects of CNWs were observed by raman spectrum. The hall measurement system was used to analyzed sheet resistance, resistivity and conductivity. The CNWs synthesized at 40 minutes showed outstanding structural and electrical characterizations than another growth times.

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.

High temperature polyimide foams for shuttle upper surface thermal insulation

NASA Technical Reports Server (NTRS)

Ball, G. L., III; Leffingwell, J. W.; Salyer, I. O.; Werkmeister, D. W.

1974-01-01

Polyimide foams developed by Monsanto Company were examined for use as upper surface space shuttle thermal insulation. It was found that postcured polyimide foams having a density of 64 kg/cu m (4 lb/cu ft) had acceptable physical properties up to and exceeding 700 K (800 F). Physical tests included cyclic heating and cooling in vacuum, weight and dimensional stability, mechanical strength and impact resistance, acoustic loading and thermal conductivity. Molding and newly developed postcuring procedures were defined.

High-precision cutting of polyimide film using femtosecond laser for the application in flexible electronics

NASA Astrophysics Data System (ADS)

Ganin, D. V.; Lapshin, K. E.; Obidin, A. Z.; Vartapetov, S. K.

2018-01-01

The experimental results of cutting a polyimide film on the optical glass substrate by means of femtosecond lasers are given. Two modes of laser cutting of this film without damages to a glass base are determined. The first is the photo graphitization using a high repetition rate femtosecond laser. The second is ablative, under the effect of femtosecond laser pulses with high energy and low repetition rate. Cutting of semiconductor chips formed on the polyimide film surface is successfully demonstrated.

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.

Polyimide foam for the thermal insulation and fire protection

NASA Technical Reports Server (NTRS)

Rosser, R. W. (Inventor)

1973-01-01

The preparation of chemically resistant and flame retardant foams from polyfunctional aromatic carboxylic acid derivatives and organic polyisocyanates is outlined. It was found that polyimide foams of reproducible density above 1 lb./ft. and below 6 lbs./cu ft. can be obtained by employing in the reaction of least 2% by weight of siloxane-glycol copolymer as a surfactant which acts as a specific density control agent. Polyimide foams into which reinforcing fibers such as silicon dioxide and carbon fibers may be incorporated were also produced.

Polyimides From BTDA, m-PDA, and HDA

NASA Technical Reports Server (NTRS)

Delano, Chadwick B.; Kiskiras, Charles J.

1987-01-01

Aliphatic segments in polyimide backbones achieve low molding temperatures and resistance to solvents. Low molding temperatures in combination with good solvent resistance make these polymers candidates for use in aerospace applications.

Progress report

NASA Technical Reports Server (NTRS)

Abhiraman, A.; Collard, D.; Cardelino, B.; Bhatia, S.; Desai, P.; Harruna, I.; Khan, I.; Mariam, Y.; Mensah, T.; Mitchell, M.

1992-01-01

The NASA funding allowed Clark Atlanta University (CAU) to establish a High Performance Polymers And Ceramics (HiPPAC) Research Center. The HiPPAC Center is consolidating and expanding the existing polymer and ceramic research capabilities at CAU through the development of interdepartmental and interinstitutional research in: (1) polymer synthesis; (2) polymer characterization and properties; (3) polymer processing; (4) polymer-based ceramic synthesis; and (5) ceramic characterization and properties. This Center has developed strong interactions between scientists and materials scientists of CAU and their counterparts from sister institutions in the Atlanta University Center (AUC) and the Georgia Institute of Technology. As a component of the center, we have started to develop strong collaborations with scientists from other universities and the HBCU's, national and federal agency laboratories, and the private sector during this first year. During this first year we have refined the focus of the research in the HiPPAC Center to three areas with seven working groups that will start programmatic activities on January 1, 1993, as follows: (1) nonlinear optical properties of chitosan derivatives; (2) polymeric electronic materials; (3) nondestructive characterization and prediction of polyimide performance; (4) solution processing of high-performance materials; (5) processable polyimides for composite applications; (6) sol-gel based ceramic materials processing; and (7) synthetic based processing of pre-ceramic polymers.

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.

Embedded Distributed Optical Fiber Sensors in Reinforced Concrete Structures—A Case Study

PubMed Central

Villalba, Sergi

2018-01-01

When using distributed optical fiber sensors (DOFS) on reinforced concrete structures, a compromise must be achieved between the protection requirements and robustness of the sensor deployment and the accuracy of the measurements both in the uncracked and cracked stages and under loading, unloading and reloading processes. With this in mind the authors have carried out an experiment where polyimide-coated DOFS were installed on two concrete beams, both embedded in the rebar elements and also bonded to the concrete surface. The specimens were subjected to a three-point load test where after cracking, they are unloaded and reloaded again to assess the capability of the sensor when applied to a real loading scenarios in concrete structures. Rayleigh Optical Frequency Domain Reflectometry (OFDR) was used as the most suitable technique for crack detection in reinforced concrete elements. To verify the reliability and accuracy of the DOFS measurements, additional strain gauges were also installed at three locations along the rebar. The results show the feasibility of using a thin coated polyimide DOFS directly bonded on the reinforcing bar without the need of indention or mechanization. A proposal for a Spectral Shift Quality (SSQ) threshold is also obtained and proposed for future works when using polyimide-coated DOFS bonded to rebars with cyanoacrylate adhesive. PMID:29587449

Embedded Distributed Optical Fiber Sensors in Reinforced Concrete Structures-A Case Study.

PubMed

Barrias, António; Casas, Joan R; Villalba, Sergi

2018-03-26

When using distributed optical fiber sensors (DOFS) on reinforced concrete structures, a compromise must be achieved between the protection requirements and robustness of the sensor deployment and the accuracy of the measurements both in the uncracked and cracked stages and under loading, unloading and reloading processes. With this in mind the authors have carried out an experiment where polyimide-coated DOFS were installed on two concrete beams, both embedded in the rebar elements and also bonded to the concrete surface. The specimens were subjected to a three-point load test where after cracking, they are unloaded and reloaded again to assess the capability of the sensor when applied to a real loading scenarios in concrete structures. Rayleigh Optical Frequency Domain Reflectometry (OFDR) was used as the most suitable technique for crack detection in reinforced concrete elements. To verify the reliability and accuracy of the DOFS measurements, additional strain gauges were also installed at three locations along the rebar. The results show the feasibility of using a thin coated polyimide DOFS directly bonded on the reinforcing bar without the need of indention or mechanization. A proposal for a Spectral Shift Quality (SSQ) threshold is also obtained and proposed for future works when using polyimide-coated DOFS bonded to rebars with cyanoacrylate adhesive.

Composite flexible blanket insulation

NASA Technical Reports Server (NTRS)

Kourtides, Demetrius A. (Inventor); Lowe, David M. (Inventor)

1994-01-01

An improved composite flexible blanket insulation is presented comprising top silicon carbide having an interlock design, wherein the reflective shield is composed of single or double aluminized polyimide and wherein the polyimide film has a honeycomb pattern.

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.

Nanotexturing of High-Performance Woven Fabrics for Novel Composite Applications

DTIC Science & Technology

2006-11-29

biocompatibility , and adhesion of dyes. At the same time the glow discharge assists in the removal of a weak boundary layer (WBL) residing on the... polyimides , polyetherimides, carbon fibers, silk, cellulose, wool, cotton, linen, etc… PLASMA ON Average process speed: 15 ft/min web width: >20 inches

The Effect of Atomic Oxygen on POSS-Polyimides (Preprint)

DTIC Science & Technology

2008-05-01

Symposium and Exhibition sponsored by the Society for the Advancement of Materials and Process Engineering, Long Beach, CA, May 12-16, 2002. 6. Koontz ...and Incoherent-Scatter Data - Msis-83," Journal of Geophysical Research-Space Physics, 1983, 88(A12), 170-188. 21. Koontz , S.L., Leger, L. J

Development of lightweight reinforced plastic laminates for spacecraft interior applications

NASA Technical Reports Server (NTRS)

Hertz, J.

1975-01-01

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

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

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

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

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

Lithium diffusion in polyether ether ketone and polyimide stimulated by in situ electron irradiation and studied by the neutron depth profiling method

NASA Astrophysics Data System (ADS)

Vacik, J.; Hnatowicz, V.; Attar, F. M. D.; Mathakari, N. L.; Dahiwale, S. S.; Dhole, S. D.; Bhoraskar, V. N.

2014-10-01

Diffusion of lithium from a LiCl aqueous solution into polyether ether ketone (PEEK) and polyimide (PI) assisted by in situ irradiation with 6.5 MeV electrons was studied by the neutron depth profiling method. The number of the Li atoms was found to be roughly proportional to the diffusion time. Regardless of the diffusion time, the measured depth profiles in PEEK exhibit a nearly exponential form, indicating achievement of a steady-state phase of a diffusion-reaction process specified in the text. The form of the profiles in PI is more complex and it depends strongly on the diffusion time. For the longer diffusion time, the profile consists of near-surface bell-shaped part due to Fickian-like diffusion and deeper exponential part.

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.

Application of polyimide actuator rod seals

NASA Technical Reports Server (NTRS)

Watermann, A. W.; Gay, B. F.; Robinson, E. D.; Srinath, S. K.; Nelson, W. G.

1972-01-01

Development of polyimide two-stage hydraulic actuator rod seals for application in high-performance aircraft was accomplished. The significant portion of the effort was concentrated on optimization of the chevron and K-section second-stage seal geometries to satisfy the requirements for operation at 450 K (350 F) with dynamic pressure loads varying between 200 psig steady-state and 1500 psig impulse cycling. Particular significance was placed on reducing seal gland dimension by efficiently utilizing the fatigue allowables of polyimide materials. Other objectives included investigation of pressure balancing techniques for first-stage polyimide rod seals for 4000 psig 450 K(350 F) environment and fabrication of a modular retainer for the two-stage combination. Seals were fabricated in 0.0254 m (1.0in.) and 0.0635 m (2.5in.) sizes and tested for structural integrity, frictional resistance, and endurance life. Test results showed that carefully designed second stages using polyimides could be made to satisfy the dynamic return pressure requirements of applications in high-performance aircraft. High wear under full system pressure indicated that further research is necessary to obtain an acceptable first-stage design. The modular retainer was successfully tested and showed potential for new actuator applications.

Positron annihilation spectroscopic study of high performance semi-interpenetrating network polyimids

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

Ray, A.K.

1995-12-01

Semi-interpenetrating (S-IPN) network polyimids were made from different proportions of LaRC RP46 (a thermosetpolyimid) and LaRC BDTA-ODA (a thermoplastic polyimid). The ultimate goal of this networking is to improve the mechanical properties of the thermoset polyimid. Positron lifetime study was made to calculate lifetime based on second component of the life time spectra and the free volume & microvoid size. All these properties tend to decrease steadily with increasing thermoset content except at the 50 percent thermoset level where these properties show sudden drop. This result contradicts with the initial expectation that the blend properties should change gradually if itmore » were a solid solution of thermoset (TSP) and thermoplastic (TPP) components. Thermal analyses (TMA, DSC, DMA & TGA) were run to complement the positron life time studies. The TMA and DSC studies confirm the contradiction mentioned above. Further experimentation with S-IPN polymers made at TSP/TTP content around 50/50 level are being conducted to explain this anomaly. Scanning electron microscope study of the S-IPN polyimid samples is under way in order to detect morphological differences which might help explain the phenomenon mentioned above.« less

Preparing thermoplastic aromatic polyimides

NASA Technical Reports Server (NTRS)

Bell, V. L.

1973-01-01

Method prepares aromatic polyimides with significantly reduced glass-transition temperatures and without accompanying loss of high-level thermo-oxidative stability which has been typical. This has been made possible by use of diamine monomers with specific stereoisomeric features.

Aromatic polyimides containing a dimethylsilane-linked dianhydride

NASA Technical Reports Server (NTRS)

St.clair, Anne K. (Inventor); St.clair, Terry L. (Inventor); Pratt, J. Richard (Inventor)

1989-01-01

A high-temperature stable, optically transparent, low dielectric aromatic polyimide is prepared by chemically combining equimolar quantities of an aromatic dianhydride reactant and an aromatic diamine reactant, which are selected so that one reactant contains at least one Si(CH3)2 group in its molecular structure, and the other reactant contains at least one -CF3 group in its molecular structure. The reactants are chemically combined in a solvent medium to form a solution of a high molecular weight polyamic acid, which is then converted to the corresponding polyimide.

Aromatic polyimides containing a dimethylsilane-linked dianhydride

NASA Technical Reports Server (NTRS)

St. Clair, Anne K. (Inventor); St. Clair, Terry L. (Inventor); Pratt, J. Richard (Inventor)

1992-01-01

A high-temperature stable, optically transparent, low dielectric aromatic polyimide is prepared by chemically combining equimolar quantities of an aromatic dianhydride reactant and an aromatic diamine reactant, which are selected so that one reactant contains at least one Si(CH.sub.3).sub.2 group in its molecular structure, and the other reactant contains at least one --CH.sub.3 group in its molecular structure. The reactants are chemically combined in a solvent medium to form a solution of a high molecular weight polyamic acid, which is then converted to the corresponding polyimide.

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.

Development of design allowable data for Celion 6000/LARC-160, graphite/polyimide composite laminates

NASA Technical Reports Server (NTRS)

Ehret, R. M.; Scanlan, P. R.; Rosen, C. D.

1982-01-01

A design allowables test program was conducted on Celion 6000/LARC-160 graphite polyimide composite to establish material performance over a 116 K (-250 F) to 589 K (600 F) temperature range. Tension, compression, in-plane shear and short beam shear properties were determined for uniaxial, quasi-isotropic and + or - 45 deg laminates. Effects of thermal aging and moisture saturation on mechanical properties were also evaluated. Celion 6000/LARC-160 graphite/polyimide can be considered an acceptable material system for structural applications to 589 K (600 F).

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.

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.

High-Solids Polyimide Precursor Solutions

NASA Technical Reports Server (NTRS)

Chuang, Chun-Hua (Inventor)

2004-01-01

The invention is a highly concentrated stable solution of polymide precursors (monometers) having a solids content ranging from about 80 to 98 percent by weight in lower aliphatic alcohols i.e. methyl and/or ethylalcohol. the concentrated polyimide precursos solution comparisons effective amounts of at least one aromatic diamine, at least one aromatic dianhydride, and a monofunctional endcap including monoamines, monoanhydrides and lower alkyl esters of said monoanhydrides. These concentrated polyimide precursor solutions are particularly useful for the preparation of fibrous prepregs and composites for use in structural materials for military and civil applications.

HPLC for quality control of polyimides

NASA Technical Reports Server (NTRS)

Young, P. R.; Sykes, G. F.

1979-01-01

High Pressure Liquid Chromatography (HPLC) as a quality control tool for polyimide resins and prepregs are presented. A data base to help establish accept/reject criteria for these materials was developed. This work is intended to supplement, not replace, standard quality control tests normally conducted on incoming resins and prepregs. To help achieve these objectives, the HPLC separation of LARC-160 polyimide precursor resin was characterized. Room temperature resin aging effects were studied. Graphite reinforced composites made from fresh and aged resin were fabricated and tested to determine if changes observed by HPLC were significant.

Tribological properties of graphite-fiber-reinforced, partially fluorinated polyimide composites

NASA Technical Reports Server (NTRS)

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

1985-01-01

Graphite-fiber-reinforced polyimide (GFRPI) composites were formulated from three new partially fluorinated polyimides and three types of graphite fiber. Nine composites were molded into pins and evaluated in a pin-on-disk tribometer. Friction coefficients, wear rates, pin wear surface morphology, and transfer film formation were assessed at 25 and 300 C. Also assessed was the effect of sliding speed on friction. Wear was up to two orders of magnitude lower at 25 C and up to one order of magnitude lower at 300 C than with previously formulated NASA GFRPI composites.

Enhanced Strain Measurement Range of an FBG Sensor Embedded in Seven-Wire Steel Strands.

PubMed

Kim, Jae-Min; Kim, Chul-Min; Choi, Song-Yi; Lee, Bang Yeon

2017-07-18

FBG sensors offer many advantages, such as a lack of sensitivity to electromagnetic waves, small size, high durability, and high sensitivity. However, their maximum strain measurement range is lower than the yield strain range (about 1.0%) of steel strands when embedded in steel strands. This study proposes a new FBG sensing technique in which an FBG sensor is recoated with polyimide and protected by a polyimide tube in an effort to enhance the maximum strain measurement range of FBG sensors embedded in strands. The validation test results showed that the proposed FBG sensing technique has a maximum strain measurement range of 1.73% on average, which is 1.73 times higher than the yield strain of the strands. It was confirmed that recoating the FBG sensor with polyimide and protecting the FBG sensor using a polyimide tube could effectively enhance the maximum strain measurement range of FBG sensors embedded in strands.

Selected fretting-wear-resistant coatings for titanium - 6-percent-aluminum - 4-percent-vanadium alloy

NASA Technical Reports Server (NTRS)

Bill, R. C.

1976-01-01

A titanium - 6-percent-aluminum - 4-percent-vanadium alloy (Ti-6Al-4V) was subjected to fretting-wear exposures against uncoated Ti-6Al-4V as a baseline and against various coatings and surface treatments applied to Ti-6Al-4V. The coatings evaluated included plasma-sprayed tungsten carbide with 12 percent cobalt, aluminum oxide with 13 percent titanium oxide, chromium oxide, and aluminum bronze with 10 percent aromatic polyester; polymer-bonded polyimide, polyimide with graphite fluoride, polyimide with molybdenum disulfide (MoS2), and methyl phenyl silicone bonded MoS2, preoxidation surface treatment, a nitride surface treatment, and a sputtered MoS2 coating. Results of wear measurements on both the coated and uncoated surfaces after 300,000 fretting cycles indicated that the polyimide coating was the most wear resistant and caused the least wear to the uncoated mating surface.

Suspension Flame Spray Construction of Polyimide-Copper Layers for Marine Antifouling Applications

NASA Astrophysics Data System (ADS)

Liu, Yi; Xu, Xiaomin; Suo, Xinkun; Gong, Yongfeng; Li, Hua

2018-01-01

Individual capsule-like polyimide splats have been fabricated by suspension flame spray, and the polyimide splat exhibits hollow structure with an inner pore and a tiny hole on its top surface. Enwrapping of 200-1000-nm copper particles inside the splats is accomplished during the deposition for constrained release of copper for antifouling performances. Antifouling testing of the coatings by 24-h exposure to Escherichia coli-containing artificial seawater shows that the Cu-doped splat already prohibits effectively attachment of the bacteria. The prohibited adhesion of bacteria obviously impedes formation and further development of bacterial biofilm. This capsulated splat with releasing and loading of copper biocides results in dual-functional structures bearing both release-killing and contact-killing mechanisms. The suspension flame spray route and the encapsulated structure of the polyimide-Cu coatings would open a new window for designing and constructing marine antifouling layers for long-term applications.

Structural and Acoustic Damping Characteristics of Polyimide Microspheres

NASA Technical Reports Server (NTRS)

Palumbo, Daniel L.; Park, Junhong

2005-01-01

A broad range of tests have been performed to evaluate the capability of tiny lightweight polyimide spheres to reduce sound and vibration. The types of testing includes impedance tube measurement of propagation constant, sound power insertion loss for single and double wall systems, particle frame wave characterization and beam vibration reduction. The tests were performed using spheres made of two types of polyimide and with varying diameter. Baseline results were established using common noise reduction treatment materials such as fiberglass and foam. The spheres were difficult to test due to their inherent mobility. Most tests required some adaptation to contain the spheres. One test returned obvious non-linear behavior, a result which has come to be expected for treatments of this type. The polyimide spheres are found to be a competent treatment for both sound and vibration energy with the reservation that more work needs to be done to better characterize the non-linear behavior.

Evaluation of two polyimides and of an improved liner retention design for self-lubricating bushings

NASA Technical Reports Server (NTRS)

Sliney, H. E.

1984-01-01

Two different polyimide polymers were studied and the effectiveness of a design feature to improve retention of the self lubricating composite liners under high load was evaluated. The basic bearing design consisted of a molded layer of chopped graphite-fiber-reinforced-polyimide (GFRP) composite bonded to the bore of a steel bushing. The friction, wear, and load carrying ability of the bushings were determined in oscillating tests at 25, 260 and 315 C at radial unit loads up to 260 MPa. Friction coefficients were typically 0.15 to 0.25. Bushings with liners containing a new partially fluorinated polymer were functional, but had a lower load capacity and higher wear rate than those containing a more conventional, high temperature polyimide. The liner retention design feature reduced the tendency of the liners to crack and work out of the contact zone under high oscillating loads.

Mechanically Resilient Polymeric Films Doped with a Lithium Compound

NASA Technical Reports Server (NTRS)

Meador, Mary Ann B. (Inventor); Kinder, James D. (Inventor)

2005-01-01

This invention is a series of mechanically resilient polymeric films, comprising rod-coil block polyimide copolymers, which are doped with a lithium compound providing lithium ion conductivity, that are easy to fabricate into mechanically resilient films with acceptable ionic or protonic conductivity at a variety of temperatures. The copolymers consists 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.

Laser direct synthesis and patterning of silver nano/microstructures on a polymer substrate.

PubMed

Liu, Yi-Kai; Lee, Ming-Tsang

2014-08-27

This study presents a novel approach for the rapid fabrication of conductive nano/microscale metal structures on flexible polymer substrate (polyimide). Silver film is simultaneously synthesized and patterned on the polyimide substrate using an advanced continuous wave (CW) laser direct writing technology and a transparent, particle-free reactive silver ion ink. The location and shape of the resulting silver patterns are written by a laser beam from a digitally controlled micromirror array device. The silver patterns fabricated by this laser direct synthesis and patterning (LDSP) process exhibit the remarkably low electrical resistivity of 2.1 μΩ cm, which is compatible to the electrical resistivity of bulk silver. This novel LDSP process requires no vacuum chamber or photomasks, and the steps needed for preparation of the modified reactive silver ink are simple and straightforward. There is none of the complexity and instability associated with the synthesis of the nanoparticles that are encountered for the conventional laser direct writing technology which involves nanoparticle sintering process. This LDSP technology is an advanced method of nano/microscale selective metal patterning on flexible substrates that is fast and environmentally benign and shows potential as a feasible process for the roll-to-roll manufacturing of large area flexible electronic devices.

Fabrication of polyimide based microfluidic channels for biosensor devices

NASA Astrophysics Data System (ADS)

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

2015-03-01

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

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

NASA Astrophysics Data System (ADS)

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

2017-04-01

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

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.

Adhesives for laminating polyimide insulated flat conductor cable

NASA Technical Reports Server (NTRS)

Montermoso, J. C.; Saxton, T. R.; Taylor, R. L.

1967-01-01

Polymer adhesive laminates polyimide-film flat conductor cable. It is obtained by reacting an appropriate diamine with a dianhydride. The adhesive has also been used in the lamination of copper to copper for the preparation of multilayer circuit boards.

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.

Honeycomb-laminate composite structure

NASA Technical Reports Server (NTRS)

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

1977-01-01

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

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.

MSFC inspections of installed polyimide wire

NASA Technical Reports Server (NTRS)

Landers, Joe C.

1994-01-01

An alert was issued because of the arc-tracking possibilities of installed polyimide wire harnesses. MSFC undertook a program to try to enhance the safety and reliability of these harnesses. Photographs are presented showing the need for inspections of installed wiring harnesses.

Polyimides Containing Amide And Perfluoroisopropyl Links

NASA Technical Reports Server (NTRS)

Dezem, James F.

1993-01-01

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

Polyimide composites: Application histories

NASA Technical Reports Server (NTRS)

Poveromo, L. M.

1985-01-01

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

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.

Synthesis and Characterization of Poly(maleic Anhydride)s Cross-linked Polyimide Aerogels

NASA Technical Reports Server (NTRS)

Guo, Haiquan; Meador, Mary Ann B.

2015-01-01

With the development of technology for aerospace applications, new thermal insulation materials are required to be flexible and capable of surviving high heat flux. For instance, flexible insulation is needed for inflatable aerodynamic decelerators which are used to slow spacecraft for entry, descent and landing (EDL) operations. Polyimide aerogels have low density, high porosity, high surface area, and better mechanical properties than silica aerogels and can be made into flexible thin films, thus they are potential candidates for aerospace needs. The previously reported cross-linkers such as octa(aminophenyl)silsesquioxane (OAPS) and 1,3,5-triaminophenoxybenzene (TAB) are either expensive or not commercially available. Here, we report the synthesis of a series of polyimide aerogels cross-linked using various commercially available poly(maleic anhydride)s, as seen in Figure 1. The amine end capped polyimide oligomers were made with 3,3,4,4-biphenyltetracarboxylic dianhydride (BPDA) and diamine combinations of dimethylbenzidine (DMBZ) and 4, 4-oxydianiline (ODA). The resulting aerogels have low density (0.12 gcm3 to 0.16 gcm3), high porosity (90) and high surface area (380-554 m2g). The effect of the different poly(maleic anhydride) cross-linkers and polyimide backbone structures on density, shrinkage, porosity, surface area, mechanical properties, moisture resistance and thermal properties will be discussed.

Evaluation of Kapton pyrolysis, arc tracking, and flashover on SiO(x)-coated polyimide insulated samples of flat flexible current carriers for Space Station Freedom

NASA Technical Reports Server (NTRS)

Stueber, Thomas J.; Mundson, Chris

1993-01-01

Kapton polyimide wiring insulation was found to be vulnerable to pyrolization, arc tracking, and flashover when momentary short-circuit arcs have occurred on aircraft power systems. Short-circuit arcs between wire pairs can pyrolize the polyimide resulting in a conductive char between conductors that may sustain the arc (arc tracking). Furthermore, the arc tracking may spread (flashover) to other wire pairs within a wire bundle. Polyimide Kapton will also be used as the insulating material for the flexible current carrier (FCC) of Space Station Freedom (SSF). The FCC, with conductors in a planar type geometric layout as opposed to bundles, is known to sustain arc tracking at proposed SSF power levels. Tests were conducted in a vacuum bell jar that was designed to conduct polyimide pyrolysis, arc tracking, and flashover studies on samples of SSF's FCC. Test results will be reported concerning the minimal power level needed to sustain arc tracking and the FCC susceptibility to flashover. Results of the FCC arc tracking tests indicate that only 22 volt amps were necessary to sustain arc tracking (proposed SSF power level is 400 watts). FCC flashover studies indicate that the flashover event is highly unlikely.

Influence of γ-Irradiation on the Optical Properties of the Polyimide-YBa2Cu3O6.7 System

NASA Astrophysics Data System (ADS)

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

2018-05-01

Influence of γ-irradiation on the optical properties of a polyimide film and its polymer compositions with fillers of a dispersed powder of a high-temperature superconductor ҮBa2Cu3O6.7 (YBaCuO) with concentrations of 0.05, 0.10, and 0.50 wt.% was studied. It was established that γ-irradiation with a dose up to 600 kGy does not affect the transparency of polyimide films in the visible region of the spectrum. However, at irradiation doses of 250 and 600 kGy, a weakly expressed fine structure appears in the spectra of polyimide films in the range of 220-300 nm due to the contribution of the resulting diene structures to the optical transmission and the increased content of oxygen atoms. The YBaCuO filler and γ-irradiation cause the polyimide transition from the amorphous state to the crystalline state, which is manifested in a sharp change in the spectrum in the range of 2.3-3.9 eV. A significant increase in the extinction coefficient was found in the composite containing 0.50 wt.% of the filler that is associated with an increase in the radius of action of structurally active fillers on the macromolecules of the matrix.

Carbon fiber on polyimide ultra-microelectrodes

NASA Astrophysics Data System (ADS)

Gillis, Winthrop F.; Lissandrello, Charles A.; Shen, Jun; Pearre, Ben W.; Mertiri, Alket; Deku, Felix; Cogan, Stuart; Holinski, Bradley J.; Chew, Daniel J.; White, Alice E.; Otchy, Timothy M.; Gardner, Timothy J.

2018-02-01

Objective. Most preparations for making neural recordings degrade over time and eventually fail due to insertion trauma and reactive tissue response. The magnitudes of these responses are thought to be related to the electrode size (specifically, the cross-sectional area), the relative stiffness of the electrode, and the degree of tissue tolerance for the material. Flexible carbon fiber ultra-microelectrodes have a much smaller cross-section than traditional electrodes and low tissue reactivity, and thus may enable improved longevity of neural recordings in the central and peripheral nervous systems. Only two carbon fiber array designs have been described previously, each with limited channel densities due to limitations of the fabrication processes or interconnect strategies. Here, we describe a method for assembling carbon fiber electrodes on a flexible polyimide substrate that is expected to facilitate the construction of high-density recording and stimulating arrays. Approach. Individual carbon fibers were aligned using an alignment tool that was 3D-printed with sub-micron resolution using direct laser writing. Indium deposition on the carbon fibers, followed by low-temperature microsoldering, provided a robust and reliable method of electrical connection to the polyimide interconnect. Main results. Spontaneous multiunit activity and stimulation-evoked compound responses with SNR  >10 and  >120, respectively, were recorded from a small (125 µm) peripheral nerve. We also improved the typically poor charge injection capacity of small diameter carbon fibers by electrodepositing 100 nm-thick iridium oxide films, making the carbon fiber arrays usable for electrical stimulation as well as recording. Significance. Our innovations in fabrication technique pave the way for further miniaturization of carbon fiber ultra-microelectrode arrays. We believe these advances to be key steps to enable a shift from labor intensive, manual assembly to a more automated manufacturing process.

Carbon fiber on polyimide ultra-microelectrodes.

PubMed

Gillis, Winthrop F; Lissandrello, Charles A; Shen, Jun; Pearre, Ben W; Mertiri, Alket; Deku, Felix; Cogan, Stuart; Holinski, Bradley J; Chew, Daniel J; White, Alice E; Otchy, Timothy M; Gardner, Timothy J

2018-02-01

Most preparations for making neural recordings degrade over time and eventually fail due to insertion trauma and reactive tissue response. The magnitudes of these responses are thought to be related to the electrode size (specifically, the cross-sectional area), the relative stiffness of the electrode, and the degree of tissue tolerance for the material. Flexible carbon fiber ultra-microelectrodes have a much smaller cross-section than traditional electrodes and low tissue reactivity, and thus may enable improved longevity of neural recordings in the central and peripheral nervous systems. Only two carbon fiber array designs have been described previously, each with limited channel densities due to limitations of the fabrication processes or interconnect strategies. Here, we describe a method for assembling carbon fiber electrodes on a flexible polyimide substrate that is expected to facilitate the construction of high-density recording and stimulating arrays. Individual carbon fibers were aligned using an alignment tool that was 3D-printed with sub-micron resolution using direct laser writing. Indium deposition on the carbon fibers, followed by low-temperature microsoldering, provided a robust and reliable method of electrical connection to the polyimide interconnect. Spontaneous multiunit activity and stimulation-evoked compound responses with SNR  >10 and  >120, respectively, were recorded from a small (125 µm) peripheral nerve. We also improved the typically poor charge injection capacity of small diameter carbon fibers by electrodepositing 100 nm-thick iridium oxide films, making the carbon fiber arrays usable for electrical stimulation as well as recording. Our innovations in fabrication technique pave the way for further miniaturization of carbon fiber ultra-microelectrode arrays. We believe these advances to be key steps to enable a shift from labor intensive, manual assembly to a more automated manufacturing process.

Semi-2-interpenetrating polymer networks of high temperature systems

NASA Technical Reports Server (NTRS)

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

1985-01-01

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

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

NASA Technical Reports Server (NTRS)

Jang, Bor Z.

1990-01-01

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

Synthesis, Processing, and Characterization of Inorganic-Organic Hybrid Cross-Linked Silica, Organic Polyimide, and Inorganic Aluminosilicate Aerogels

NASA Technical Reports Server (NTRS)

Nguyen, Baochau N.; Guo, Haiquan N.; McCorkle, Linda S.

2014-01-01

As aerospace applications become ever more demanding, novel insulation materials with lower thermal conductivity, lighter weight and higher use temperature are required to fit the aerospace application needs. Having nanopores and high porosity, aerogels are superior thermal insulators, among other things. The use of silica aerogels in general is quite restricted due to their inherent fragility, hygroscopic nature, and poor mechanical properties, especially in extereme aerospace environments. Our research goal is to develop aerogels with better mechanical and environmental stability for a variety of aeronautic and space applications including space suit insulation for planetary surface missions, insulation for inflatable structures for habitats, inflatable aerodynamic decelerators for entry, descent and landing (EDL) operations, and cryotank insulation for advance space propulsion systems. Different type of aerogels including organic-inorganic polymer reinforced (hybrid) silica-based aerogels, polyimide aerogels and inorganic aluminosilicate aerogels have been developed and examined.

Anisotropic Copoly(Imide Oxetane) Coatings and Articles of Manufacture, Copoly(Imide Oxetane)s Containing Pendant Fluorocarbon Moieties, Oligomers and Processes Therefor

NASA Technical Reports Server (NTRS)

Wohl, Christopher J. (Inventor); Siochi, Emilie J. (Inventor); Smith, Joseph G. (Inventor); Connell, John W. (Inventor)

2017-01-01

Copoly(imide oxetane) materials are disclosed that can exhibit a low surface energy while possessing the mechanical, thermal, chemical and optical properties associated with polyimides. The copoly(imide oxetane)s are prepared using a minor amount of fluorinated oxetane-derived oligomer with sufficient fluorine-containing segments of the copoly(imide oxetane)s that migrate to the exterior surface of the polymeric material to yield low surface energies. Thus the coatings and articles of manufacture made with the copoly(imide oxetane)s of this invention are characterized as having an anisotropic fluorine composition. The low surface energies can be achieved with very low content of fluorinated oxetane-derived oligomer. The copolymers of this invention can enhance the viability of polyimides for many applications and may be acceptable where homopolyimide materials have been unacceptable.

Development and investigation of flexible polymer neural probe for chronic neural recording

NASA Astrophysics Data System (ADS)

Smith, Courtney; Song, Kyo D.; Yoon, Hargsoon; Kim, Woong-Ki; Zeng, Tao; Sanford, Larry D.

2012-04-01

Neural recording through microelectrodes requires biocompatibility and long term chronic usage. With a potential for various applications and effort to improve the performance of neural recording probes, consideration is taken to the tissue and cellular effects in these device designs. The degeneration of neurons due to brain tissue motion is an issue along with brain tissue inflammation in the insertion of the probes. To account for motion and irritation the material structure of the probes must be improved upon. This research presents the fabrication of neural probes on the microscale utilizing flexible polymers. Polyimide neural probes have been considered possibly to reduce degradation in their variability caused by brain motion. The microfabrication of the polyimide neural probe has an increased flexibility while accounting for biocompatibility and the needs for chronic use. Through microfabrication processes a needle probe is produced and tested for neural recording.

Keeping Cool in Extreme Heat

NASA Technical Reports Server (NTRS)

2001-01-01

Through a partnership with Unitika Ltd., NASA's Langley Research Center created a foam based on high temperature resistant polyimide chemistry. Licensed non-exclusively to SORDAL, Inc., the low-density foam, named TEEK, can be processed into forms or used to fill structures such as honeycomb. TEEK offers superior insulation and support qualities, with heat and flame resistance abilities.TEEK is a practical selection for hull insulation in the shipbuilding industry, with numerous potential applications in aerospace applications, fire-resistant construction materials, and a wide range of consumer products that will improve safety and energy efficiency. Other opportunities are available in the areas of automotive coatings and sealants, electrical components, and recreational equipment. SORDAL has introduced its new product in several different forms, under the name "SOLREX". The company is developing a new product called SORDAL Paper(TM) that will be used in conjunction with the polyimide foam to offer thermal protection in various products, such as fire resistant garments and prosthetics.

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.

Polyimides Derived from Novel Asymmetric Dianhydrides

NASA Technical Reports Server (NTRS)

Chuang, Chun-Hua (Inventor)

2012-01-01

This invention relates to the compositions and processes for preparing thermoset and thermoplastic polyimides derived from novel asymmetrical dianhydrides: specifically 2,3,3',4' benzophenone dianhydride (a-BTDA), and 3,4'-(hexafluoroisopropylidene)diphthalic anhydride (a-6FDA). The a-BTDA anhydride is prepared by Suzuki coupling with catalysts from a mixed anhydride of 3,4-dimethylbenzoic acid or 2,3-dimethylbenzoic acid with 2,3-dimethylphenylboronic acid or 3,4-dimethylphenylboronic acid respectively, to form 2,3,3',4'-tetramethylbenzophenone which is oxidized to form 2,3,3',4'-benzophenonetetracarboxylic acid followed by cyclodehydration to obtain a-BTDA. The a-6FDA is prepared by nucleophilic triflouoromethylation of 2,3,3',4'-tetramethylbenzophenone with trifluoromethyltrimethylsilane to form 3,4'-(trifluoromethylmethanol)-bis(o-xylene) which is converted to 3,4'-(hexafluoroisopropylidene-bis(o-xylene). The 3,4'-(hexafluoroisopropylidene)-bis(o-xylene) is oxidized to the corresponding tetraacid followed by cyclodehydration to yield a-6FDA.

Antifouling enhancement of polyimide membrane by grafting DEDA-PS zwitterions.

PubMed

Zhang, Dong Yan; Xiong, Shu; Shi, Yu Sheng; Zhu, Jun; Hu, Qiao Li; Liu, Jie; Wang, Yan

2018-05-01

In order to improve the water flux and antifouling property of polyimide (PI) membrane, zwitterions are grafted on PI membrane surface via a two-step modification route by reactions with N,N-diethylethylenediamine (DEDA) and 1,3-propane sultone (PS) sequentially. The reaction mechanism and physicochemical properties of membranes are confirmed via various characterization techniques. The anti-biofouling performance of the zwitterion-grafted PI membranes is evaluated by bacterial suspension immersion tests in Escherichia coli (E. coli) and staphylococcus aureus (S. aureus) solutions. The antifouling property is assessed via the filtration test using the bovine serum albumin (BSA) and dodecyl trimethyl ammonium bromide (DTAB) aqueous feed solutions. The effect of the reaction time with DEDA in the zwitterion-grafted process on the antifouling property is further investigated systematically. The results show that both the anti-biofouling and antifouling performances of zwitterion-grafted PI membranes are significantly improved. Copyright © 2018 Elsevier Ltd. All rights reserved.

Interlaminar fracture toughness of thermoplastic composites

NASA Technical Reports Server (NTRS)

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

1988-01-01

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

Effect of Sizings on the Durability of High Temperature Polymer Composites

NASA Technical Reports Server (NTRS)

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

2003-01-01

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

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.

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

NASA Technical Reports Server (NTRS)

Alston, William B.

1988-01-01

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

Design and fabrication of micro-hotplates made on a polyimide foil: electrothermal simulation and characterization to achieve power consumption in the low mW range

NASA Astrophysics Data System (ADS)

Courbat, J.; Canonica, M.; Teyssieux, D.; Briand, D.; de Rooij, N. F.

2011-01-01

The design of ultra-low power micro-hotplates on a polyimide (PI) substrate supported by thermal simulations and characterization is presented. By establishing a method for the thermal simulation of very small scale heating elements, the goal of this study was to decrease the power consumption of PI micro-hotplates to a few milliwatts to make them suitable for very low power applications. To this end, the mean heat transfer coefficients in air of the devices were extracted by finite element analysis combined with very precise thermographic measurements. A simulation model was implemented for these hotplates to investigate both the influence of their downscaling and the bulk micromachining of the polyimide substrate to lower their power consumptions. Simulations were in very good agreement with the experimental results. The main parameters influencing significantly the power consumption at such dimensions were identified and guidelines were defined allowing the design of very small (15 × 15 µm) and ultra-low power heating elements (6 mW at 300 °C). These very low power heating structures enable the realization of flexible sensors, such as gas, flow or wind sensors, for applications in autonomous wireless sensors networks or RFID applications and make them compatible with large-scale production on foil such as roll-to-roll or printing processes.

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.

Development of High Performance Piezoelectric Polyimides

NASA Technical Reports Server (NTRS)

Simpson, Joycelyn O.; St.Clair, Terry L.; Welch, Sharon S.

1996-01-01

In this work a series of polyimides are investigated which exhibit a strong piezoelectric response and polarization stability at temperatures in excess of 100 C. This work was motivated by the need to develop piezoelectric sensors suitable for use in high temperature aerospace applications.

Compounds containing meta-biphenylenedioxy moieties and polymers therefrom

NASA Technical Reports Server (NTRS)

St.clair, Terry L. (Inventor); Pratt, John Richard (Inventor)

1993-01-01

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 prepare polyimide polymers. These polymers are used to make films, coatings, and selective membranes.

Design Analysis and Thermo-Mechanical Fatigue of a Polyimide Composite for Combustion Chamber Support

NASA Technical Reports Server (NTRS)

Thesken, J. C.; Melis, M.; Shin, E.; Sutter, J.; Burke, Chris

2004-01-01

Polyimide composites are being evaluated for use in lightweight support structures designed to preserve the ideal flow geometry within thin shell combustion chambers of future space launch propulsion systems. Principles of lightweight design and innovative manufacturing techniques have yielded a sandwich structure with an outer face sheet of carbon fiber polyimide matrix composite. While the continuous carbon fiber enables laminated skin of high specific stiffness; the polyimide matrix materials ensure that the rigidity and durability is maintained at operation temperatures of 316 C. Significant weight savings over all metal support structures are expected. The protypical structure is the result of ongoing collaboration, between Boeing and NASA-GRC seeking to introduce polyimide composites to the harsh environmental and loads familiar to space launch propulsion systems. Design trade analyses were carried out using relevant closed form solutions, approximations for sandwich beams/panels and finite element analysis. Analyses confirm the significant thermal stresses exist when combining materials whose coefficients of thermal expansion (CTEs) differ by a factor of about 10 for materials such as a polymer composite and metallic structures. The ramifications on design and manufacturing alternatives are reviewed and discussed. Due to stringent durability and safety requirements, serious consideration is being given to the synergistic effects of temperature and mechanical loads. The candidate structure operates at 316 C, about 80% of the glass transition temperature T(sub g). Earlier thermomechanical fatigue (TMF) investigations of chopped fiber polyimide composites made this near to T(sub g), showed that cyclic temperature and stress promoted excessive creep damage and strain accumulation. Here it is important to verify that such response is limited in continuous fiber laminates.

High density circuit technology

NASA Technical Reports Server (NTRS)

Wade, T. E.

1979-01-01

Polyimide dielectric materials were acquired for comparative and evaluative studies in double layer metal processes. Preliminary experiments were performed. Also, the literature indicates that sputtered aluminum films may be successfully patterned using the left-off technique provided the substrate temperature remains low and the argon pressure in the chamber is relatively high at the time of sputtering. Vendors associated with dry processing equipment are identified. A literature search relative to future trends in VLSI fabrication techniques is described.

Processable high temperature resistant polymer matrix materials

NASA Technical Reports Server (NTRS)

Serafini, T. T.

1975-01-01

A review is presented of studies conducted with addition-cured polyimides, giving particular attention to an improved method involving in situ polymerization of monomer reactants (PMR) on the surface of the reinforcing fibers. The studies show that the PMR approach provides a powerful method for fabricating high performance polymer matrix composites. Significant advantages of the PMR approach are related to the superior high temperature properties of the obtained material, lower cost, greater safety, and processing versatility.

Study of two different thin film coating methods in transmission laser micro-joining of thin Ti-film coated glass and polyimide for biomedical applications.

PubMed

Sultana, T; Georgiev, G L; Baird, R J; Auner, G W; Newaz, G; Patwa, R; Herfurth, H J

2009-07-01

Biomedical devices and implants require precision joining for hermetic sealing which can be achieved with low power lasers. The effect of two different thin metal film coating methods was studied in transmission laser micro-joints of titanium-coated glass and polyimide. The coating methods were cathodic arc physical vapor deposition (CA-PVD) and electron beam evaporation (EB-PVD). Titanium-coated glass joined to polyimide film can have neural electrode application. The improvement of the joint quality will be essential for robust performance of the device. Low power fiber laser (wave length = 1100 nm) was used for transmission laser micro-joining of thin titanium (Ti) film (approximately 200 nm) coated Pyrex borosilicate 7740 glass wafer (0.5 mm thick) and polyimide (Imidex) film (0.2 mm thick). Ti film acts as the coupling agent in the joining process. The Ti film deposition rate in the CA-PVD was 5-10 A/s and in the EB-PVD 1.5 A/s. The laser joint strength was measured by a lap shear test, the Ti film surfaces were analyzed by atomic force microscopy (AFM) and the lap shear tested joints were analyzed by optical microscopy and scanning electron microscopy (SEM). The film properties and the failure modes of the joints were correlated to joint strength. The CA-PVD produced around 4 times stronger laser joints than EB-PVD. The adhesion of the Ti film on glass by CA-PVD is better than that of the EB-PVD method. This is likely to be due to a higher film deposition rate and consequently higher adhesion or sticking coefficient for the CA-PVD particles arriving on the substrate compared to that of the EB-PVD film. EB-PVD shows poor laser bonding properties due to the development of thermal hotspots which occurs from film decohesion.

Polyimide Foams Offer Superior Insulation

NASA Technical Reports Server (NTRS)

2012-01-01

At Langley Research Center, Erik Weiser and his colleagues in the Advanced Materials and Processing Branch were working with a new substance for fabricating composites for use in supersonic aircraft. The team, however, was experiencing some frustration. Every time they tried to create a solid composite from the polyimide (an advanced polymer) material, it bubbled and foamed. It seemed like the team had reached a dead end in their research - until they had another idea. "We said, This isn t going to work for composites, but maybe we could make a foam out of it," Weiser says. "That was kind of our eureka moment, to see if we could go in a whole other direction. And it worked." Weiser and his colleagues invented a new kind of polyimide foam insulation they named TEEK. The innovation displayed a host of advantages over existing insulation options. Compared to other commercial foams, Weiser explains, polyimide foams perform well across a broad range of temperatures, noting that the NASA TEEK foams provide effective structural insulation up to 600 F and down to cryogenic temperatures. The foam does not burn or off-gas toxic fumes, and even at -423 F - the temperature of liquid hydrogen - the material stays flexible. The inventors could produce the TEEK foam at a range of densities, from 0.5 pounds per cubic foot up to 20 pounds per cubic foot, making the foam ideal for a range of applications, including as insulation for reusable launch vehicles and for cryogenic tanks and lines. They also developed a unique, friable balloon format for manufacturing the foam, producing it as hollow microspheres that allowed the foam to be molded and then cured into any desired shape - perfect for insulating pipes of different sizes and configurations. The team s originally unplanned invention won an "R&D 100" award, and a later form of the foam, called LaRC FPF-44 (Spinoff 2009), was named "NASA Invention of the Year" in 2007.

Characterization of Polyimide Foams for Ultra-Lightweight Space Structures

NASA Technical Reports Server (NTRS)

Meador, Michael (Technical Monitor); Hillman, Keithan; Veazie, David R.

2003-01-01

Ultra-lightweight materials have played a significant role in nearly every area of human activity ranging from magnetic tapes and artificial organs to atmospheric balloons and space inflatables. The application range of ultra-lightweight materials in past decades has expanded dramatically due to their unsurpassed efficiency in terms of low weight and high compliance properties. A new generation of ultra-lightweight materials involving advanced polymeric materials, such as TEEK (TM) polyimide foams, is beginning to emerge to produce novel performance from ultra-lightweight systems for space applications. As a result, they require that special conditions be fulfilled to ensure adequate structural performance, shape retention, and thermal stability. It is therefore important and essential to develop methodologies for predicting the complex properties of ultra-lightweight foams. To support NASA programs such as the Reusable Launch Vehicle (RLV), Clark Atlanta University, along with SORDAL, Inc., has initiated projects for commercial process development of polyimide foams for the proposed cryogenic tank integrated structure (see figure 1). Fabrication and characterization of high temperature, advanced aerospace-grade polyimide foams and filled foam sandwich composites for specified lifetimes in NASA space applications, as well as quantifying the lifetime of components, are immensely attractive goals. In order to improve the development, durability, safety, and life cycle performance of ultra-lightweight polymeric foams, test methods for the properties are constant concerns in terms of timeliness, reliability, and cost. A major challenge is to identify the mechanisms of failures (i.e., core failure, interfacial debonding, and crack development) that are reflected in the measured properties. The long-term goal of the this research is to develop the tools and capabilities necessary to successfully engineer ultra-lightweight polymeric foams. The desire is to reduce density at the material and structural levels, while at the same time maintaining or increasing mechanical and other properties.

Enhanced Strain Measurement Range of an FBG Sensor Embedded in Seven-Wire Steel Strands

PubMed Central

Kim, Jae-Min; Kim, Chul-Min; Choi, Song-Yi

2017-01-01

FBG sensors offer many advantages, such as a lack of sensitivity to electromagnetic waves, small size, high durability, and high sensitivity. However, their maximum strain measurement range is lower than the yield strain range (about 1.0%) of steel strands when embedded in steel strands. This study proposes a new FBG sensing technique in which an FBG sensor is recoated with polyimide and protected by a polyimide tube in an effort to enhance the maximum strain measurement range of FBG sensors embedded in strands. The validation test results showed that the proposed FBG sensing technique has a maximum strain measurement range of 1.73% on average, which is 1.73 times higher than the yield strain of the strands. It was confirmed that recoating the FBG sensor with polyimide and protecting the FBG sensor using a polyimide tube could effectively enhance the maximum strain measurement range of FBG sensors embedded in strands. PMID:28718826

Investigation of the interfacial reaction between metal and fluorine-contained polyimides

NASA Astrophysics Data System (ADS)

Yang, Ching-Yu; Chen, J. S.; Hsu, S. L. C.

2005-07-01

In this work, thin metal films (Cr and Ta) were deposited on fluorine-contained polyimides, 6FDA-BisAAF, and 6FDA-PPD. The chemical states of the metal/polyimide samples were characterized by using x-ray photoelectron spectroscopy (XPS). XPS analysis reveals that metal-C, C-O, and metal-O bondings are present in metallized 6FDA-BisAAF and 6FDA-PPD. C-F bonds are observed in bare 6FDA-BisAAF and 6FDA-PPD however, they are not seen in the metallized samples. Disappearance of the C-F bonding is attributed to the disruption of CF3 side groups from the main chains of 6FDA-BisAAF and 6FDA-PPD when the chains are exposed to the plasma during the metal deposition. Nevertheless, the disruption of CF3 side groups also creates sites for the formation of metal-C or C-O bondings, which provide a positive adhesion strength at the metal/polyimide interface, as revealed by the tape test.