Layered silicate nanocomposites based on various high-functionality epoxy resins. Part II: The influence of an organoclay on the rheological behavior of epoxy prepolymers

The effect of an organically surface modified layered silicate on the viscosity of various epoxy resins of different structures and different functionalities was investigated. Steady and dynamic shear viscosities of the epoxy resins containing 0-10 wt% of the organoclay were determined using parallel plate rheology. Viscosity results were compared with those achieved through addition of a commonly used micron-sized CaCO3 filler. It was found that changes in viscosities due to the different fillers were of the same order, since the layered silicate was only dispersed on a micron-sized scale in the monomer (prior to reaction), as indicated by X-ray diffraction measurements. Flow activation energies at a low frequency were determined and did not show any significant changes due to the addition of organoclay or CaCO3. Comparison between dynamic and steady shear experiments showed good agreement for low layered silicate concentrations below 7.5 wt%, i.e. the Cox-Merz rule can be applied. Deviations from the Cox-Merz rule appeared at and above 10 wt%, although such deviations were only slightly above experimental error. Most resin organoclay blends were well predicted by the Power Law model, only concentrations of 10 wt% and above requiring the Herschel-Buckley (yield stress) model to achieve better fits. Wide-angle X-ray measurements have shown that the epoxy resin swells the layered silicate with an increase in the interlayer distance of approximately 15 Angstrom, and that the rheology behavior is due to the lateral, micron-size of these swollen tactoids.

Layered silicate nanocomposites based on various high-functionality epoxy resins: The influence of an organoclay on resin cure

The influence of an organically modified clay on the curing behavior of three epoxy systems widely used in the aerospace industry and of different structures and functionalities, was studied. Diglycidyl ether of bisphenol A (DGEBA), triglycidyl p-amino phenol (TGAP) and tetraglycidyl diamino diphenylmethane (TGDDM) were mixed with an octadecyl ammonium ion modified organoclay and cured with diethyltoluene diamine (DETDA). The techniques of dynamic mechanical thermal analysis (DMTA), chemorheology and differential scanning calorimetry (DSC) were applied to investigate gelation and vitrification behavior, as well as catalytic effects of the clay on resin cure. While the formation of layered silicate nanocomposite based on the bifunctional DGEBA resin has been previously investigated to some extent, this paper represents the first detailed study of the cure behavior of different high performance, epoxy nanocomposite systems.

The effect of a curing agent on the thermal degradation of fire retardant brominated epoxy resins

The diglycidyl ether of tetrabromobisphenol A, the diglycidyl ether of bisphenol A and their mixture was cured by 4,4'-diaminodiphenyl methane. The pyrolysis of the obtained epoxy resins was studied by TG, DSC, TG/FTIR as well as FTIR characterization of pyrolysis residues. The gaseous and high boiling pyrolysis products were collected, characterized by GC/MS and their formation is discussed. The brominated epoxy resins are thermally less stable than the non-brominated ones. This effect is caused by the amine-containing hardener. The degradation initiation reaction is associated with the formation of hydrogen bromide which further destabilizes the epoxy network. The effect of the curing agent can be used in recycling of epoxy resins to separate brominated pyrolysis products from non-brominated ones.

Study on microwave dielectric properties of epoxy resin mixtures used for rapid product development

This paper presents a preliminary study on the dielectric properties and curing of three different types of epoxy resins mixed at various stichiometric mixture of hardener, flydust and aluminium powder under microwave energy. In this work, the curing process of thin layers of epoxy resins using microwave radiation was investigated as an alternative technique that can be implemented to develop a new rapid product development technique. In this study it was observed that the curing time and temperature were a function of the percentage of hardener and fillers presence in the epoxy resins. Initially dielectric properties of epoxy resins with hardener were measured which was directly correlated to the curing process in order to understand the properties of cured specimen. Tensile tests were conducted on the three different types of epoxy resins with hardener and fillers. Modifying dielectric properties of the mixtures a significant decrease in curing time was observed. In order to study the microstructural changes of cured specimen the morphology of the fracture surface was carried out by using scanning electron microscopy.

New Energetic Epoxy Binders

A new class of epoxy resins having N-N bonds in the backbone has been synthesized with a view to explore their properties as energetic binders. The N-epoxidation of bis-dicarbonylhydrazones of adipic, azelaic and sebacic dihydrazides results in the formation of viscous resins having epoxide end groups. The resins have been characterized by the elemental and end group analyses, IR and NMR spectra. Relevant properties for their use as binders in solid propellants, such as thermal stability, heat of combustion, burn rate and performance parameters of AP-based propellant systems, have been evaluated. A significant increase in the burn rate of AP-based propellants noticed, is perhaps related to the exothermicity of the binder decomposition and the reactivity of N-N bonds with perchloric acid formed during the combustion of AP.

Alumina and Silica based Epoxy Nano-composites for Electrical Insulation

Plain epoxy resins or resin impregnated cellulose have found application as electrical insulation in power equipment. In the past, their performance was improved by the use of inorganic oxide fillers of microscopic dimensions. In the recent past nano-particle doped epoxy insulation came into use with a view to further enhance the dielectric properties. This paper reports dielectric investigations into epoxy nano-composites based on a class of metal oxides, Al2O3 and SiO2. In particular, consideration has been given to the partial discharge performance and electrical breakdown under different voltage profiles as a function of the volumetric composition of the nano-particles in epoxy resin.

PHASE-BEHAVIOR IN EPOXY-RESIN CONTAINING PHENOLPHTHALEIN POLY(ETHER ETHER SULFONE)

Phenolphthalein poly(ether ether sulphone) (PES-C) was found to be miscible with uncured bisphenol-A-type epoxy resin, i.e. diglycidyl ether of bisphenol A (DGEBA), as shown by the existence of a single glass transition temperature within the whole composition range. Miscibility between PES-C and DGEBA is considered to be due mainly to the entropy contribution. However, dynamic mechanical analysis (d.m.a.) and scanning electron microscopy (SEM) studies revealed that PES-C exhibits different miscibility with four cured epoxy resins (ER). The overall compatibility and the resulting morphology of the cured blends are dependent on the choice of cure agent. For the blends cured with amines (4,4'-diaminodiphenylmethane (DDM) and 4,4'-diaminodiphenylsulphone (DDS)), no phase separation occurs as indicated by either d.m.a. or SEM. However, for the blends cured with anhydrides (maleic anhydride (MA) and phthalic anhydride (PA)), both d.m.a. and SEM clearly show evidence of phase separation. SEM study shows that the two phases interact well in the MA-cured blend while the interface between the phases in the PA-cured blend is poorly bonded. The differences in the overall compatibility and the resulting morphology between the amine-cured and anhydride-cured systems have been discussed from the points of view of both thermodynamics and kinetics.

Isora Fibre Reinforced Polyester and Epoxy Composites

The aim of this investigation is to study the effectiveness of isora fibre as reinforcement material in short and long forms, for unsaturated polyester and epoxy resins.Studies on the optimization of fibre length and fibre loading of randomly oriented isora-polyester composite are described.The salient features of the alkali treatment of short isora fibre on the properties of randomly oriented isora-polyester composite are outlined in this thesis.The effect of surface modification of the hydrophilic isora fibre by different chemical treatments on the properties of randomly oriented isora-polyester composite is outlined.The properties of oriented and randomly oriented isora fibre reinforced epoxy composites with special reference to the effect of fibre loading are reported and also the dynamic mechanical properties ofthe oriented and randomly oriented isora-polyester and isora-epoxy composites are presented and the water absorption kinetics of oriented and randomly oriented isora-polyester composites and oriented isoraepoxy composites are given. The effect of hot air oven aging on the tensile and flexural properties of oriented isora-polyester and isora-epoxy composites are also reported in this thesis.

Epoxy-modiWed, unsaturated polyester hybrid networks

Hybrid polymer networks (HPNs) based on unsaturated polyester resin (UPR) and epoxy resins were synthesized by reactive blending. The epoxy resins used were epoxidised phenolic novolac (EPN), epoxidised cresol novolac (ECN) and diglycidyl ether of bisphenol A (DGEBA). Epoxy novolacs were prepared by glycidylation of the novolacs using epichlorohydrin. The physical, mechanical, and thermal properties of the cured blends were compared with those of the control resin. Epoxy resins show good miscibility and compatibility with the UPR resin on blending and the co-cured resin showed substantial improvement in the toughness and impact resistance. Considerable enhancement of tensile strength and toughness are noticed at very low loading of EPN. Thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA) and diVerential scanning calorimetry (DSC) were employed to study the thermal properties of the toughened resin. The EPN/ UPR blends showed substantial improvement in thermal stability as evident from TGA and damping data. The fracture behaviour was corroborated by scanning electron microscopy (SEM). The performance of EPN is found to be superior to other epoxy resins

Modifications of DGEBA Using Epoxidised Resins

Modifications of DGEBA Using Epoxidised Resins

Structural and material properties of a rapidly cured thermoplastic-toughened epoxy system

Thermoplastic-toughened epoxy resins are widely used as matrices in modern composite prepreg systems. Rapid curing of thermoplastic-toughened epoxy matrix composites results in different mechanical properties. To investigate the structure–property relationship, we investigated a poly(ether sulfone)-modified triglycidylaminophenol/ 4,4'-diamino diphenyl sulfone system that was cured at different heating rates. An intermediate dwell was also applied during the rapid heating of the thermoplasticmodified epoxy system. We found that a higher heating rate led to a larger domain size of the phase-separated macrostructure and also facilitated more complete phase separation. The intermediate dwell helped phase separation to proceed even further, leading to an even larger domain size of the macrostructure. A carbon-fiber-reinforced polymer matrix composite prepreg based on the poly(ether sulfone)-modified multifunctional epoxy system was cured with the same schedule. The rapidly heated composite laminates exhibited higher mode I delamination fracture toughness than the slowly heated material.

Structure and properties of epoxy nanocomposites

This study investigated the structure-property relationships of epoxy nanocomposites when processing the materials under various conditions. A sonication technique, rapid heating rate and mechanical vibration during curing facilitated the dispersion of nanoclay in an epoxy resin. This led to the successful manufacture of fibre reinforced nanocomposites.

A systematic study of carbon fibre surface grafting via in situ diazonium generation for improved interfacial shear strength in epoxy matrix composites

A recently established means of surface functionalization of unsized carbon fibres for enhanced compatibility with epoxy resins was optimised and evaluated using interfacial shear stress measurements. Interfacial adhesion has a strong influence on the bulk mechanical properties of composite materials. In this work we report on the optimisation of our aryl diazo-grafting methodology via a series of reagent concentration studies. The fibres functionalised at each concentration are characterised physically (tensile strength, modulus, coefficient of friction, and via AFM), and chemically (XPS). The interfacial shear strength (IFSS) of all treated fibres was determined via the single fibre fragmentation test, using the Kelly-Tyson model. Large increases in IFSS for all concentrations (28-47%) relative to control fibres were observed. We show that halving the reagent concentration increased the coefficient of friction of the fibre and the interfacial shear strength of the composite while resulting in no loss of the key performance characteristics in the treated fibre.

Hygrothermal effects on damping behavior of metal/glass fiber/epoxy hybrid composites

Continuous fiber/metal laminates (FML) offer significant improvements over current available materials for aircraft structures due to their excellent fatigue endurance and low density. Glass fibers/epoxy laminae and aluminum foil (Glare) are commonly used to obtain these hybrid composites. The environmental factors can limit the applications of composites by deteriorating the mechanical properties during service. Usually, epoxy resins absorb moisture when exposed to humid environments and metals are prone to surface corrosion. Therefore, the combination of the two materials in Glare (polymeric composite and metal). can lead to differences that often turn out to be beneficial in terms of mechanical properties and resistance to environmental influences. In this work. The viscoelastic properties. such as storage modulus (E') and loss modulus (E'), were obtained for glass fiber/epoxy composite, aluminum 2024-T3 alloy and for a glass fiber/epoxy/aluminum laminate (Glare). It was found that the glass fiber/epoxy (G/E) composites decrease the E' modulus during hygrothermal conditioning up to saturation point (6 weeks). However, for Glare laminates the E' modulus remains unchanged (49GPa) during the cycle of hygrothermal conditioning. The outer aluminum sheets in the Glare laminate shield the G/E composite laminae from moisture absorption. which in turn prevent, in a certain extent, the material from hygrothermal degradation effects. (c) 2005 Elsevier B.V. All rights reserved.

Characterization of cure of carbon/epoxy prepreg used in aerospace field

Carbon/epoxy 8552 prepreg is a thermoplastic toughened high-performance epoxy being used in the manufacture of advanced army material. Understanding the cure behavior of a thermosetting system is essential in the development and optimization of composite fabrication processes. The cure kinetics and rheological behavior were evaluated using a differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA) and a rheometer. Values of the kinetic parameters were obtained from dynamic DSC scans using an nth order reaction model. Rheological measurements as a function of temperature and time were made for the prepreg system. The manufacturer's recommended cure cycle was evaluated and considered adequate to consolidated the studied system.