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At least 217 records · Page 12

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NASA NTRS1989

ESR Measurement Of Crystallinity In Semicrystalline Polymers

Photogenerated free radicals decay at different rates in crystalline and amorphous phases. Degree of crystallinity in polymer having both crystalline and amorphous phases measured indirectly by technique based in part on electron-spin-resonance (ESR) spectroscopy. Accuracy of crystallinity determined by new technique equals or exceeds similar determinations by differential scanning calorimetry, wide-angle x-ray scattering, or measurement of density.

Kim, Soon Sam↗

NASA NTRS1988

Isomeric oxydiphthalic anhydride polyimides

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.

Gerber, Margaret K.↗

NASA NTRS1988

Fire and heat resistant laminating resin based on maleimido and citraconimido substituted 1-(diorganooxyphosphonyl-methyl)-2,4- and -2,6-diaminobenzenes

The subject invention pertains to a novel class of fire-and heat-resistant bisimide resins prepared by thermal polymerization of maleimido or citraconimido substituded 1-(dialkoxyphosphonyl)-methyl-2-4 and -2,6-diaminobenzenes. Typical polymer presursors have the chemical structure wherein R is alkyl, substituted alkyl or aryl, and R sup 1 is hydrogen or lower alkyl. The polymer precursors are prepared by reacting 1-(diorganooxyphosphonyl)methyl-2-4 and -2,6-diaminobenzenes with maleic anhydride or citraconic anhydride in a mole ratio 1:2. Chains extension of the monomers is achieved by reacting the mono-N-maleimido derivatives of 1-(diorganooxyphosphonyl)methyl-2,4 and -2,6-diaminobenzenes with aryl tetracarboxylic dianhydrides, such as benzophenone tetracarboxylic diandydride, or aryl diisocyanates, such as methylenebis (4-phenylisocyanate), in a mole ratio 2:1. The polymerization of the monomers is studied by differential scanning calorimetry (DSC) and the thermal stability of the polymers is ascertained by thermogravimetric analysis (TGA).

James M Beggs↗

NASA NTRS1988

A study of thermal transitions in a new semicrystalline thermoplastic polyimide

A polyimide derive from 4,4'-isophthaloyl diphthalic anhydride (IDPA) and 1,3-bis (4-aminophenoxy 4'-benzoyl) benzene (1,3-BABB) having semicrystalline behavior was prepared and characterized by differential scanning calorimetry (DSC) and wide angle X-ray scattering (WAXS). Thus a poly(amic acid) film cured in air for one hour each at 100 and 200 C displayed an endotherm at 286 C, followed by a crystallization exotherm at 317 C, and a second melting transition at 350 C. The 286 C melting point appeared to result from earlier solvent-induced crystallization. Films cast from DMAc, air dried, and soaked in methylene chloride could not be induced into semicrystallinity. The fully cured polyimide has a Tg of 216 C. Films heated to temperatures as high as 100 C for one hour in air were transparent and light yellow in color. Those films heated to or above 125 C were translucent. Polarized light microscopy revealed the presence of spherulites 608 micrometers in diameter in a sample cured to 275 C in air. Two film samples, one cured to 275 and the other to 325 C, were evaluated for tensile and ultimate strength, modulus, and percent elongation at 25 and 200 C. These values remained essentially constant at each test temperature.

Pratt, J. Richard↗

NASA NTRS1988

Crystallization of BaF2-ZnF2-YbF3-ThF4 glass

The phases and the rates of crystallization in a Ba-Zn-Yb-Th fluoride glass were studied using differential scanning calorimetry, XRD, and observational and chemical SEM analyses. The crystallizing phases that were identified included a BaYbTh fluoride, ZnF2, and YbF3. The BaYbTh fluoride crystallized first at about 450 C, and ZnF2, which was excluded from this phase, crystallized at its surfaces. At higher temperatures, the BaYbTh fluoride phase decomposed partially to BaThF6 and YbF3 phases.

Garcia, Roberto↗

NASA NTRS1988

The glass transition, crystallization and melting in Au-Pb-Sb alloys

The glass transition, crystallization and melting of Au(55)Pb(22.5)Sb(22.5) alloys have been studied by differential scanning calorimetry DSC. Crystallization on heating above the glass transition temperature Tg (45 C) begins at 64 C. Further crystallization events are observed at 172 C and 205 C. These events were found to correspond to the formation of the intermetallic compounds AuSb2, Au2Pb, and possibly AuPb2, respectively. Isothermal DSC scans of the glassy alloy above Tg were used to monitor the kinetics of crystallization. The solidification behavior and heat capacity in the glass-forming composition range were determined with droplet samples. An undercooling level of 0.3T(L) below the liquidus temperature T(L) was achieved, resulting in crystallization of different stable and metastable phases. The heat capacity C(P) of the undercooled liquid was measured over an undercooling range of 145 C.

Lee, M. C.↗

NASA NTRS1988

Annealing study of poly(etheretherketone)

Annealing of PEEK has been studied for two materials cold-crystallized from the rubbery amorphous state. The first material is a low molecular weight PEEK; the second is commercially available neat resin. Differential scanning calorimetry was used to monitor the melting behavior of annealed samples. The effect of thermal history on melting behavior is very complex and depends upon annealing temperature, residence time at the annealing temperature, and subsequent scanning rate. Thermal stability of both materials is improved by annealing, and for an annealing temperature near the melting point, the polymer can be stabilized against reorganization during the scan. Variations of density, degree of crystallinity, and X-ray long period were studied as a function of annealing temperature for the commercial material.

Cebe, Peggy↗

NASA NTRS1988

High resolution X-ray spectroscopy using microcalorimeters

The use of microcalorimeters for high-resolution, high quantum efficiency, nondispersive X-ray spectroscopy has been demonstrated over the past few years. In this paper, the principles of X-ray calorimetry are reviewed, and the results of ongoing X-ray tests using microcalorimetry are summarized. An approach to building an X-ray calorimeter spectrometer is discussed.

Kelley, R. L.↗

NASA NTRS1989

Investigations of microwave plasmas - Applications in electrothermal thruster systems

Experimental studies which have been conducted to develop understanding of plasma processes used for spacecraft propulsion are reviewed. The techniques discussed are calorimetry and volume measurements using the TM 011 and TM 012 modes in the microwave cavity system. The use of plasmas in electrical propulsion and microwave induction is reviewed. Plasma containment, microwave power production, energy distribution, and the pressure and flow dependence of the energy distribution are addressed. The plasma dimensions and their dependence on pressure, flow, and power are considered.

Haraburda, Scott S.↗

NASA NTRS1989

Superconducting ceramics in the Bi1.5SrCaCu2O sub x system by melt quenching technique

Bi sub 1.5 SrCaCu sub 2 O sub x has been prepared in the glassy state by rapid quenching of the melt. The kinetics of crystallization of various phases in the glass have been evaluated by a variable heating rate differential scanning calorimetry method. The formation various phases on thermal treatments of the glass has been investigated by powder X-ray diffraction and electrical resistivity measurements. Heating at 450 C formed Bi sub 2 Sr sub 2 CuO sub 6, which disappeared on further heating at 765 C, where Bi sub 2 Sr sub 2 CaCu sub 2 O sub 8 formed. Prolonged heating at 845 C resulted in the formation of a small amount of a phase with T sub c onset of approx. 108 K, believed to be Bi sub 2 Sr sub 2 Ca sub 2 Cu sub 3 O sub 10. This specimen showed zero resistivity at 54 K. The glass ceramic approach could offer several advantages in the fabrication of the high-T sub c superconductors in desired practical shapes such as continuous fibers, wires, tapes, etc.

Bansal, Narottam P.↗

NASA NTRS1989

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

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).

Pratt, J. Richard↗

NASA NTRS1990

LaRC TPI 1500 series polymers

The crystallization behavior and the melt flow properties of two batches of 1500 series LaRC-TPI polymers from Mitsui Toatsu Chemicals (MTC) were investigated. The characterization methods include Differential Scanning Calorimetry, the x ray diffractography and the melt rheology. The as-received materials possess initial crystalline melting peak temperatures of 295 and 305 C, respectively. These materials are less readily recrystallizable at elevated temperatures when compared to other semicrystalline thermoplastics. For the samples annealed at temperatures below 330 C, a semicrystalline polymer can be obtained. On the other hand, a purely amorphous structure is realized in the samples annealed at temperatures above 330 C. Isothermal crystallization kinetics were studied by means of the simple Avrami equation. The viscoelastic properties at elevated temperatures below and above glass transition temperature of the polymers were measured. Information with regard to the molecule sizes and distributions in these polymers were also extracted from melt rheology.

Hou, Tan-Hung↗

NASA NTRS1990

The effects of zinc addition on the environmental stability of Al-Li alloys

It was found that relatively small addition of Zn can improve the stress corrosion cracking (SCC) resistance of Al-Li alloys. However, the mechanism by which this is accomplished is unclear. The role that Zn plays in altering the behavior of Alloy 8090 is investigated. Early results suggest that Zn additions increase the volume fraction of delta(Al3Li) precipitation and differential scanning calorimetry (DSC) on these alloys confirms this. The four alloys studied each had initial compositions lying in the 8090 window and had varying amounts of Zn added to them. Alloy 8090, like other Al-Li alloys, displays a delta' precipitate free zone (PFZ) upon artificial aging along the grain and subgrain boundaries. However Zn additions greatly decreased or eliminated a delta' PFZ after 100 hours at 160 C. This implies that the subgrain boundary precipitation kinetics are being altered and suppressed. Furthermore, there appears to be a window of Zn concentration above which a delta ' PFZ can reappear with the nucleation and growth of a currently unidentified precipitate on the boundaries. Polarization experiments were performed and the results presented. The experiments were performed in deaerated 3.5 w/o NaCl in both as received (T3) condition and at peak aging of 100 hours at 160 C. The aging profile was determined via Vickers Hardness tests.

Kilmer, Raymond J.↗

NASA NTRS1989

Non-ideality near the monotectic composition of a miscibility-gap type system - Succinonitrile-water

Differential scanning calorimetry (DSC) of near monotectic succinonitrile-water solutions, fast-quenched in hydrophilic and hydrophobic DSC pans, indicate, by degree of undercooling, thst there may be significant dependence of final ingot microstructure on the pre-quench equilibration temperature. Partial molal-volume determinations from density data, along with DSC data, suggest the nature of temperature dependent component associations from 20 to 55 C in homogeneous solutions. The undercooling profile in a hydrophilic container is explained in terms of solution-composition shifts arising from the Gibbs surface excess. The evidence shows that temperature-dependent preferred component aggregates may modulate surface-composition gradients. Similar effects may be present through intermetallic compound formation in metallic monotectic alloys.

Frazier, D. O.↗

NASA NTRS1989

Effect of heat-treatment temperature of vapor-grown graphite fibers. I - Properties of their bromine intercalation compounds

Vapor-grown graphite fibers were heat treated at 2000, 2200, 2400, 2600, 2800, and 3000 C, brominated at room temperature for two days, and then characterized by X-ray diffraction analysis, differential scanning calorimetry, and resistivity measurements. Fibers greater than 13 microns in diameter had low resistivities (50 microohms or less) irrespective of the heat treatment temperature. An analysis of the results obtained suggests that resistivities below 6 microohms cannot be achieved through a further reduction in defect level unless the amount of bromine is increased.

Gaier, James R.↗

NASA NTRS1990

Characterization of two germania gels of different coordination

Two germania gels were synthesized by hydrolytic condensation of germanium ethoxide and by dissolution of germanium dioxide powder in ammonium hydroxide solution. The two gels were characterized using differential scanning calorimetry, X-ray powder diffraction, surface area and weight loss data, and infrared spectroscopy. The results indicate that, in gels, germanium is capable of tetragonal as well as hexagonal coordination, resulting in different crystallization behaviors.

Mukherjee, Shyama P.↗

NASA NTRS1990

Polyamideimides containing carbonyl and ether connecting groups

Polyamidenimides were prepared from the reaction of trimellitic anhydride chloride with seven diamines containing carbonyl and ether groups between the aromatic rings. Several of these polyamideimides were semicrystalline as evidenced by wide-angle X-ray diffraction and differential scanning calorimetry. Glass transition temperatures ranged between 187 and 245 C, and crystalline transition temperatures ranged between 317 and 416 C. A series of copolyamideimides from a mixture of 1,3-bis(4-aminophenoxy 4-prime-benzoyl) benzene and 1,4-bis(4-aminophenoxy 4-prime-benzoyl)benzene were similarly prepared. These copolyamideimides were semicrystalline and formed tough, solvent resistant films with good tensile properties.

Havens, S. J.↗

NASA NTRS1991

Correlating DSC and X-Ray Measurements Of Crystallinity

Experiment demonstrated approximate linear correlation between degree of crystallinity of multiphase polymer (as calculated from x-ray diffraction measurements) and heat of fusion of polymer (as calculated from differential scanning calorimetry (DSC) measurements). Correlation basis of simple new technique for estimating degree of crystallinity of specimens of polymer from DSC measurements alone.

Yen, Shiao-Ping S.↗