Kinetic equation parameters for the curing reaction of a commercial glass fiber reinforced high performance epoxy prepreg composed of the tetrafunctional epoxy tetraglycidyl 4,4-diaminodiphenyl methane (TGDDM), the tetrafunctional amine curing agent 4,4'-diaminodiphenylsulfone (DDS) and an ionic initiator/accelerator, are determined by various thermal analysis techniques and the results compared. The reaction is monitored by heat generated determined by differential scanning calorimetry (DSC) and by high speed DSC when the reaction rate is high. The changes in physical properties indicating increasing conversion are followed by shifts in glass transition temperature determined by DSC, temperature-modulated DSC (TMDSC), step scan DSC and high speed DSC, thermomechanical (TMA) and dynamic mechanical (DMA) analysis and thermally stimulated depolarization (TSD). Changes in viscosity, also indicative of degree of conversion, are monitored by DMA. Thermal stability as a function of degree of cure is monitored by thermogravimetric analysis (TGA). The parameters of the general kinetic equations, including activation energy and rate constant, are explained and used to compare results of various techniques. The utilities of the kinetic descriptions are demonstrated in the construction of a useful time-temperature-transformation (TTT) diagram and a continuous heating transformation (CHT) diagram for rapid determination of processing parameters in the processing of prepregs. Shrinkage due to both resin consolidation and fiber rearrangement is measured as the linear expansion of the piston on a quartz dilatometry cell using TMA. The shrinkage of prepregs was determined to depend on the curing temperature, pressure applied and the fiber orientation. Chemical modification of an epoxy was done by mixing a fluorinated aromatic amine (aniline) with a standard aliphatic amine as a curing agent for a commercial Diglycidylether of Bisphenol-A (DGEBA) epoxy. The resulting cured network was tested for wear resistance using tribological techniques. Of the six anilines, 3-fluoroaniline and 4-fluoroaniline were determined to have lower wear than the unmodified epoxy, while the others showed much higher wear rates.

Kinetic equation parameters for the curing reaction of a commercial glass fiber reinforced high performance epoxy prepreg composed of the tetrafunctional epoxy tetraglycidyl 4,4-diaminodiphenyl methane (TGDDM), the tetrafunctional amine curing agent 4,4’-diaminodiphenylsulfone (DDS) and an ionic initiator/accelerator, are determined by various thermal analysis techniques and the results compared. The reaction is monitored by heat generated determined by differential scanning calorimetry (DSC). The changes in physical properties indicating increasing conversion are followed by shifts in glass transition temperature determined by DSC and temperature-modulated DSC (TMDSC), thermomechanical (TMA) and dynamic mechanical (DMA) analysis and thermally stimulated depolarization (TSD). Changes in viscosity, also indicative of degree of conversion, are monitored by DMA. Thermal stability as a function of degree of cure is monitored by thermogravimetric analysis (TGA). The parameters of the general kinetic equations, including activation energy and rate constant, are explained and used to compare results of various techniques. The utilities of the kinetic descriptions are demonstrated in the construction of a useful time-temperature-transformation (TTT) diagram for rapid determination of processing parameters in the processing of prepregs. Copyright is held by the author, unless otherwise noted. All rights reserved. Files: Thesis.pdf Special Conditions

Star-like lignin-poly(propylene oxide) copolymers were prepared by chain-extending steam exploded lignins (tulipifera liriodendron) with propylene oxide and by subsequent endcapping with ethylene oxide. Epoxidation of these copolymers was carried out with epichlorohydrin at room temperature, using KOH as oxyanion forming reagent. The epoxidized compounds were fractionated by solvent precipitation to remove poly(alkylene oxide) homopolymers and to prepare fractions of narrow molecular weight distributions. The epoxides were cross-linked with meta phenylene diamine yielding thermosets which were, depending on lignin content, either low modulus elastomers, or high modulus materials with considerable ductility. The modulus of elasticity was a strong and linear function of lignin content, whereby the highest value was 1100MPa (57% lignin). The curing reaction was of nth-order type, whereby the reaction order changed from close to one at the beginning of the curing reaction to 2, once the reaction becomes diffusion controlled. Curing induced partial demixing of the lignin and poly(propylene oxide) phases which yielded a secondary structure where lignin rich domains in the order of 10 nm were interspersed in a matrix of lignin poor material. However, from TEM and ¹³C solid state cross-polarized NMR analyses it was evident that the domain structure was not that of a classical micro-phase separated copolymer with well defined phase boundaries, but rather had broad interphases. Additionally, the results of multifrequency dynamic mechanical thermal analysis showed that the lignin containing thermosets have very broad glass transition ranges which most likely were due to transitional phase inhomogeneities and provided these materials with good vibrational damping ability. / Ph. D.

The purpose of this study was to determine the effect of exposure conditions, resin composition, and resin treatment on film formation on metal surfaces exposed to epoxy resin. Epoxy rods were prepared from novolac hardened by 4-4' methylenedianiline (MDA). The curing and post curing temperatures were 60, 125 °C and 125, 160 °C. The composition of the epoxies used were 27.0 and 31. 5 parts (MDA) per 100 parts epoxy. The metals investigated were pure gold, silver, and copper; gold-copper alloys; gold-silver alloys; and electroformed gold-copper alloys. The alloys ranged in composition from 75 to 92 per cent gold. These samples were cleaned, weighed, placed in individual, covered, glass containers with the epoxy rods, and then were exposed at 30, 60, and 90 °C. The change in weight of the metal samples was determined at intervals of about. 30 days for five months. Weight increases of 0.1 to 0.4 milligram were observed for the samples exposed to the epoxy rods, and were negligible for samples stored without epoxy rods. The contaminating materials, apparently, are organic compounds consisting of unreacted monomer and degradation products. The film forms from a heavy, stagnant, low-lying, vapor-phase from the epoxy, with the vapors adsorbed or reacted on the surface of the metal samples. Film formation is not affected to any appreciable extent by the combined effect of increased curing temperatures and increased hardener content. The effect of increasing the temperature from 30 °C to 60 or 90 °C, on the rate of film formation was inconclusive. Epoxy film formation was observed on all metal samples tested, pure gold, copper, and silver; gold-copper and gold-silver alloys. The metal composition affects the rate of film formation with the rate increasing with decreased golJ composition for both copper and silver alloys. / Master of Science

Thesis (Elec.E)--Massachusetts Institute of Technology, Dept. of Electrical Engineering and Computer Science, 1982. / MICROFICHE COPY AVAILABLE IN ARCHIVES AND ENGINEERING / Includes bibliographical references. / by Huan Lim Lee. / Elec.E

Thesis (M.S.)--University of Michigan, 1988.

Thesis (M.S.)--University of Michigan, 1988.

No description available.

This research deals with the mechanical characterisation of thick composite laminates in the through-thickness direction. Three independent glass fibre/epoxy laminate configurations, namely cross, quasi-isotropic, and woven, plies were investigated. Six specimen configurations, of which two were developed herein, were employed in order to determine the strength behaviour of these three laminate configurations when subjected to interlaminar shear and interlaminar tensile stresses in isolation and in combination. The stress and strain distributions were estimated using the ABAQUS FEA package. The strain distribution obtained thereby was verified experimentally via Moirandeacute; interferometry which records the exact strain field at the test section. A two dimensional failure envelope is defined for each laminate configuration using the experimentally obtained data. All three independent laminate configurations exhibited almost identical failure envelopes. The woven laminate exhibited superior interlaminar shear strength when subjected to combined interlaminar shear and interlaminar tensile stresses, whereas the cross-ply laminate exhibited superior interlaminar tensile strength when subjected to the same combination of stress. The characteristics of the quasi-isotropic laminate were similar to that of the cross-ply laminate. A partial three dimensional failure envelope was also defined for the materials tested.

The effects of octadecylamine-functionalized reduced graphene oxide (FRGO) on the frictional and wear properties of diglycidylether of bisphenol-A (DGEBA) epoxy are studied using a pin-on-disk tribometer. It was observed that the addition of FRGO significantly improves the tribological, mechanical, and thermal properties of epoxy matrix. Graphene oxide (GO) was functionalized with octadecylamine (ODA), and then reduction of oxygen-containing functional groups was carried out using hydrazine monohydrate. The Raman and x-ray photoelectron spectroscopy studies confirm significant reduction in oxygen-containing functional groups and formation of ODA functionalized reduced GO. The nanocomposites are prepared by adding 0.1, 0.2, 0.5 and 1.0 wt % of FRGO to the epoxy. The addition of FRGO increases by more than an order of magnitude the sliding distance during which the dynamic friction is ≤ 0.1. After this distance, the friction sharply increases to the range of 0.4 - 0.5. We explain the increase in sliding distance during which the friction is low by formation of a transfer film from the nanocomposite to the counterface. The wear rates in the low and high friction regimes are approximately 1.5 x 10-4 mm3/N·m and 5.5 x 10-4 mm3/N·m, respectively. The nanocomposites exhibit a 74 % increase in Young’s modulus with 0.5 wt. % of FRGO, and an increase in glass transition and thermal degradation temperatures.