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NASA NTRS1993

Crystallization of copper metaphosphate glass

The effect of the valence state of copper in copper metaphosphate glass on the crystallization behavior and glass transition temperature has been investigated. The crystallization of copper metaphosphate is initiated from the surface and its main crystalline phase is copper metaphosphate (Cu(PO)3),independent of the (Cu sup 2+)/(Cu(total)). However, the crystal morphology, the relative crystallization rates, and their temperature dependences are affected by the (Cu sup 2+)/(Cu (total)) ratio in the glass. On the other hand, the totally oxidized glass crystallizes from all over the surface. The relative crystallization rate of the reduced glass to the totally oxidized glass is large at low temperature, but small at high temperature. The glass transition temperature of the glass increases as the (Cu sup 2+)/(Cu(total)) ratio is raised. It is also found that the atmosphere used during heat treatment does not influence the crystallization of the reduced glass, except for the formation of a very thin CuO surface layer when heated in air.

Bae, Byeong-Soo↗

NASA NTRS2003

Failure Criterion For Isotropic Time Dependent Materials Which Accounts for Multi-Axial Loading

The Space Shuttle's Reusable Solid Rocket Motor (RSRM) nozzle program has recently conducted testing to characterize the effects of multi-axial loading, temperature and time on the failure characteristics of TIGA321, EA913NA, EA946 (three filled epoxy adhesives). From the test data a "Multi-Axial, Temperature, and Time Dependent" or MATT failure criterion was developed. It is shown that this criterion simplifies, for constant load and constant load rate conditions, into a form that can be easily used for stress analysis. Failure for TIGA321 and EA913NA are characterized below their glass transition temperature. Failure for EA946 is characterized for conditions that pass through its glass transition. The MATT failure criterion is shown to be accurate for a wide range of conditions for these adhesives.

Richardson, D. E.↗

NASA NTRS1974

Isothermal transitions of a thermosetting system

A study of the curing reactions of a cycloaliphatic epoxy resin/anhydride system by torsional braid analysis showed the existence of two critical isothermal temperatures - namely, the maximum glass transition temperature of the thermoset system and the glass transition temperature of the material at its gel point. Two rheologically active kinetic transitions occur during isothermal cure which correspond to gelation and vitrification. Three types of isothermal behavior occur. Methods for determining the time to gel and the time to vitrify, and also the two above-mentioned critical isothermal temperatures, have been developed. The time to gel obeyed the Arrhenius relationship, whereas the time to vitrify passed through a minimum. Application of these results to thermosetting systems in general is discussed in terms of the influence of molecular structure on the values of the critical isothermal temperatures.

Gillham, J. K.↗

NASA NTRS1991

Applying state diagrams to food processing and development

The physical state of food components affects their properties during processing, storage, and consumption. Removal of water by evaporation or by freezing often results in formation of an amorphous state (Parks et al., 1928; Troy and Sharp, 1930; Kauzmann, 1948; Bushill et al., 1965; White and Cakebread, 1966; Slade and Levine, 1991). Amorphous foods are also produced from carbohydrate melts by rapid cooling after extrusion or in the manufacturing of hard sugar candies and coatings (Herrington and Branfield, 1984). Formation of the amorphous state and its relation to equilibrium conditions are shown in Fig. 1 [see text]. The most important change, characteristic of the amorphous state, is noticed at the glass transition temperature (Tg), which involves transition from a solid "glassy" to a liquid-like "rubbery" state. The main consequence of glass transition is an increase of molecular mobility and free volume above Tg, which may result in physical and physico-chemical deteriorative changes (White and Cakebread, 1966; Slade and Levine, 1991). We have conducted studies on phase transitions of amorphous food materials and related Tg to composition, viscosity, stickiness, collapse, recrystallization, and ice formation. We have also proposed that some diffusion-limited deteriorative reactions are controlled by the physical state in the vicinity of Tg (Roos and Karel, 1990, 1991a, b, c). The results are summarized in this article, with state diagrams based on experimental and calculated data to characterize the relevant water content, temperature, and time-dependent phenomena of amorphous food components.

Non-NASA Center↗

NASA NTRS2003

Multiaxial Temperature- and Time-Dependent Failure Model

A temperature- and time-dependent mathematical model predicts the conditions for failure of a material subjected to multiaxial stress. The model was initially applied to a filled epoxy below its glass-transition temperature, and is expected to be applicable to other materials, at least below their glass-transition temperatures. The model is justified simply by the fact that it closely approximates the experimentally observed failure behavior of this material: The multiaxiality of the model has been confirmed (see figure) and the model has been shown to be applicable at temperatures from -20 to 115 F (-29 to 46 C) and to predict tensile failures of constant-load and constant-load-rate specimens with failure times ranging from minutes to months..

Richardson, David↗

NASA NTRS1983

Crystal nucleation in amorphous (Au/100-y/Cu/y/)77Si9Ge14 alloys

Because, unlike most metallic glasses, melt-spun alloys of the series (Au/100-y/Cu/y/)77Si9Ge14 exhibit well separated glass transition and kinetic crystallization temperatures, crystallization can be studied in the fully relaxed amorphous phase. An isothermal calorimetric analysis of the devitrification kinetics of the amorphous alloy indicates sporadic nucleation and a constant growth rate. It is found for the cases of alloys with y values lower than 25 that the classical theory of homogeneous nucleation is consistent with observations, including transient effects. An analysis of the crystallization kinetics shows that slow crystal growth rates play an important role in glass formation in these alloys. Although the reduced glass transition temperature increases with Cu content, glass formation is more difficult at high Cu contents, perhaps because of a difference in nucleus composition.

Thompson, C. V.↗

NASA NTRS1976

Investigation of structure-property relationships in systematic series of novel polymers

Solid state transitions in polymeric materials was associated with the onset of sub-molecular motions of the polymer chains. Although these were considered to be intramolecular in general, the local environment of the polymer molecule exerts a strong influence through, for example, the effects of crystallinity, polarity and diluents. The manner of specimen preparation and previous history also affect transitions. The transitions are considered to arise when sufficient free volume is available to permit the occurrence of these side chain and backbone reorientations. The glass transition is the principal transition of amorphous polymeric materials and is associated with the onset of long range segmental motion of the polymer backbone. The various types of shorter range motion occurring below the glass transition have been catalogued.

Gillham, J. K.↗

NASA NTRS2005

Verification of the Multi-Axial, Temperature and Time Dependent (MATT) Failure Criterion

An extensive test and analytical effort has been completed by the Space Shuttle's Reusable Solid Rocket Motor (KSKM) nozzle program to characterize the failure behavior of two epoxy adhesives (TIGA 321 and EA946). As part of this effort, a general failure model, the "Multi-Axial, Temperature, and Time Dependent" or MATT failure criterion was developed. In the initial development of this failure criterion, tests were conducted to provide validation of the theory under a wide range of test conditions. The purpose of this paper is to present additional verification of the MATT failure criterion, under new loading conditions for the adhesives TIGA 321 and EA946. In many cases, the loading conditions involve an extrapolation from the conditions under which the material models were originally developed. Testing was conducted using three loading conditions: multi-axial tension, torsional shear, and non-uniform tension in a bondline condition. Tests were conducted at constant and cyclic loading rates ranging over four orders of magnitude. Tests were conducted under environmental conditions of primary interest to the RSRM program. The temperature range was not extreme, but the loading ranges were extreme (varying by four orders of magnitude). It should be noted that the testing was conducted at temperatures below the glass transition temperature of the TIGA 321 adhesive. However for the EA946, the testing was conducted at temperatures that bracketed the glass transition temperature.

Richardson, David E.↗

NASA NTRS1995

Composite prepreg application device

A heated shoe and cooled pressure roller assembly for composite prepreg application is provided. The shoe assembly includes a heated forward contact surface having a curved pressure surface. The following cooled roller provides a continuous pressure to the thermoplastic while reducing the temperature to approximately 5 C below glass transition temperature. Electric heating coils inside the forward portion of the shoe heat a thermoplastic workpiece to approximately 100 C above the glass transition. Immediately following the heated contact surface, a cooled roller cools the work. The end sharpened shape of the heated shoe trailing edge tends to prevent slag buildup and maintain a uniform, relaxed stress fabrication.

Sandusky, Donald A.↗

NASA NTRS1996

Composite prepreg application device

A heated shoe and cooled pressure roller assembly for composite prepreg application is provided. The shoe assembly includes a heated forward contact surface having a curved pressure surface. The following cooled roller provides a continuous pressure to the thermoplastic while reducing the temperature to approximately 5.degree. C. below glass transition temperature. Electric heating coils inside the forward portion of the shoe heat a thermoplastic workpiece to approximately 100.degree. C. above the glass transition. Immediately following the heated contact surface, a cooled roller cools the work. The end sharpened shape of the heated shoe trailing edge tends to prevent slag buildup and maintain a uniform, relaxed stress fabrication.

Sandusky, Donald A.↗

NASA NTRS1989

Temperature Dependence Of Elastic Constants Of Polymers

Two papers extend theory of elastic constants of disordered solids to finite temperatures below glass-transition temperatures. First paper, entitled "Elastic Constants of Disordered Solids II: Temperature Dependence," applies to cryogenic temperatures. Second paper, entitled "Theory of Thermoelastic Properties for Polymer Glasses," develops unified treatment for static compressional and elongational properties at temperatures up to glass-transition temperatures.

Simha, Robert↗

NASA NTRS1991

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

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

Roberts, Gary D.↗

NASA NTRS2003

Polyimides by Photochemical Cyclopolymerization

The polyimides of this invention are derived from a Diels-Alder cyclopolymerization of a photochemically generated bisdiene with dienophiles, such as bismaleimides, trismaleimides and mixtures thereof with maleimide end-caps. Irradiation of one or more diketones produces two distinct hydroxy o-quinodimethane (photoenol) intermediates. These intermediates are trapped via a Diels-Alder cycloaddition with appropriate dienophiles, e.g., bismaleimide and/or trismaleimides to give the corresponding polyimides in quantitative yields. When bismaleimides, trismaleimides or mixtures thereof with maleimide end-caps are used as the dienophile, the resulting polyimides have glass transition temperatures (Tg) as high as 300 C. Polyimide films can be prepared by ultraviolet irradiation of high solids content varnishes of the monomers in a small amount of solvent, e.g., cyclohexanone, dimethyl formamide, N-methylpyrollidone and the like. These polyimides are characterized as having high glass transition temperatures, good mechanical properties and improved processing in the manufacture of adhesives, electronic materials and films.

Michael A Meador↗

NASA NTRS2005

Polyimides by Photochemical Cyclopolymerization

The novel polyimides of this invention are derived from Diels-Alder cyclopolymerization of photochemically generated bisdienes with dienophiles, such as bismaleimides, trismaleimides and mixtures thereof with maleimide endcaps. Irradiation of one or more diketones produces two distinct hydroxy o-quinodimethane (photoenol) intermediates. These intermediates are trapped via Diels-Alder cycloaddition with appropriate dienophiles, e.g., bismaleimide and/or trismaleimides to give the corresponding polyimides in quantitative yields. When bismaleimides, trismaleimides or mixtures thereof with maleimide end-caps are used as the dienophile, the resulting polyimides have glass transition temperatures (Tg) as high as 300 C. Polyimide films can be prepared by ultraviolet irradiation of high solids content varnishes of the monomers in a small amount of solvent, e.g., cyclohexanone, dimethyl formamide, N-methylpyrollidone and the like. These novel polyimides are characterized as having high glass transition temperatures, good mechanical properties and improved processing in the manufacture of adhesives, electronic materials and films.

Meador, Michael A.↗

NASA NTRS2005

Polyimides by photochemical cyclopolymerization

The novel polyimides of this invention are derived from Diels-Alder cyclopolymerization of photochemically generated bisdienes with dienophiles, such as bismaleimides, trismaleimides and mixtures thereof with maleimide end-caps. Irradiation of one or more diketones produces two distinct hydroxy o-quinodimethane (photoenol) intermediates. These intermediates are trapped via Diels-Alder cycloaddition with appropriate dienophiles, e.g., bismaleimide and/or trismaleimides to give the corresponding polyimides in quantitative yields. When bismaleimides, trismaleimides or mixtures thereof with maleimide end-caps are used as the dienophile, the resulting polyimides have glass transition temperatures (Tg) as high as 300? C. Polyimide films can be prepared by ultraviolet irradiation of high solids content varnishes of the monomers in a small amount of solvent, e.g., cyclohexanone, dimethyl formamide, N-methylpyrollidone and the like. These novel polyimides are characterized as having high glass transition temperatures, good mechanical properties and improved processing in the manufacture of adhesives, electronic materials and films.

Meador, Michael A.↗

NASA NTRS2002

Polyesters by Photochemical Cyclopolymerization

The polyesters of this invention are derived from a Diels-Alder cyclopolymerization of a photochemically generated bisdiene with dienophiles, such as di(acrylates), tri (acrylates), di(methacrylates), tri(methacrylates) and mixtures thereof with mono(methacrylates) or mono(acrylate) end-caps. Irradiation of one or more diketones produces two distinct hydroxy o-quinodimethane (photoenol) intermediates. These intermediates are trapped via a Diels-Alder cycloaddition with appropriate dienophiles, e.g., di(acrylates) to give the corresponding in polyesters quantitative yields. When di(acrylates), tri(acrylates) and di and tri(methacrylates) or mixtures thereof with monoacrylate end-caps are used as the dienophile, the resulting polyesters have glass transition temperatures (Tg) as high as 200 C. Polyesters films can be prepared by ultraviolet irradiation of high solids content varnishes of the monomers in a small amount of solvent, e.g., cyclohexanone, dimethyl formamide, N-methylpyrollidone and the like. These polyesters, i.e. polyesters are characterized as having high glass transition temperatures, good mechanical properties and improved processing in the manufacture of composites, adhesives, electronic materials and films.

Michael A Meador↗

NASA NTRS1997

Liquid water in the domain of cubic crystalline ice Ic

Vapor-deposited amorphous water ice when warmed above the glass transition temperature (120-140 K), is a viscous liquid which exhibits a viscosity vs temperature relationship different from that of liquid water at room temperature. New studies of thin water ice films now demonstrate that viscous liquid water persists in the temperature range 140-210 K. where it coexists with cubic crystalline ice. The liquid character of amorphous water above the glass transition is demonstrated by (1) changes in the morphology of water ice films on a nonwetting surface observed in transmission electron microscopy (TEM) at around 175 K during slow warming, (2) changes in the binding energy of water molecules measured in temperature programmed desorption (TPD) studies, and (3) changes in the shape of the 3.07 micrometers absorption band observed in grazing angle reflection-absorption infrared spectroscopy (RAIRS) during annealing at high temperature. whereby the decreased roughness of the water surface is thought to cause changes in the selection rules for the excitation of O-H stretch vibrations. Because it is present over such a wide range of temperatures, we propose that this form of liquid water is a common material in nature. where it is expected to exist in the subsurface layers of comets and on the surfaces of some planets and satellites.

NASA Center ARC↗

NASA NTRS1994

Effect Of Molecular Weight On Adhesive Properties Of The Phenylethynyl-Terminated Polyimide LARC(sup TM)-PETI-5

Future civilian aircraft will require the use of advanced adhesive systems with high temperature capabilities. One such material has been developed at the NASA Langley Research Center, a phenylethynyl-terminated polyimide given the designation LARC(sup TM)-PETI-5. Recent work has shown the advantages of similar phenylethynyl-terminated polyimides as films, moldings, adhesives, and composite matrix resins. Phenylethynyl-terminated oligomers provide greater processing windows than materials which incorporate simple ethynyl endcaps. Since these low molecular weight, low melt viscosity oligomers thermally cure without the evolution of volatile by-products, they provide an excellent means of producing polymers with high glass transition temperatures, excellent solvent resistance, and high mechanical properties. Three different versions of LARC(sup TM)-PETI-5 with theoretical number average molecular weights (M(sub n)s) of 250, 5000, and 10000 g/mol were synthesized in this work. Differential Scanning Calorimetry (DSC) measurements were performed on the dry powder form of these materials to establish cure conditions which result in high glass transition temperatures (T(sub g)s). Lap shear specimens were prepared from adhesive tape made from each material and with the thermal cure conditions determined from the DSC data. The tensile shear data established processing conditions which provided the best adhesive strengths. Further testing was performed to establish the properties of LARC(sup TM)-PETI-5 as an adhesive material and to determine its solvent resistance.

Cano, Roberto J.↗