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At least 19 records

Reliable Bonding of Composite Laminates Using Reflowable Epoxy Resins

Epoxy matrix composites assembled with adhesives maximize the performance of aerospace structures, but the possibility of forming weak bonds requires the installation of redundant fasteners, which add weight and manufacturing cost. Co-cured joints (e.g. unitized composite structures) are immune to weak bonds because the uncured resin undergoes diffusion and mixing through the joint. A means of co-curing complex structures may reduce the need for redundant fasteners in bondlines. To this end, NASA started the AERoBOND project to develop novel joining materials to enable a “secondary-co-cure” assembly process. Aerospace epoxy resin systems reformulated with offset stoichiometry prevented the resin from advancing beyond the gel point during a conventional autoclave cure cycle up to 180 °C. The offset resins were applied to the joining surfaces of laminate preforms as prepreg. Two surfaces with complimentary offset resins were joined using conventional secondary bonding techniques. Preliminary efforts have indicated that the resulting joint has no discernable interface and appears as a conventional co-cured laminate under optical magnification. This report will discuss the initial work performed regarding formulation of the epoxy resin system using calorimetry, rheology, and mechanical testing.

Palmieri, Frank L.

Morphology and properties of amine terminated poly(arylene ether ketone) and poly(arylene ether sulfone) modified epoxy resin systems

Epoxy resin networks cured with DDS were modified by incorporating tough ductile thermoplastics such as the amine terminated polyether sulfones and amine terminated polyether ketones. Both linear copolymers were able to significantly improve the fracture toughness values at the 15 and 30 weight percent concentrations examined. These improvements in fracture toughness were achieved without any significant change in the flexural modulus.

Cecere, J. A.

Poly(arylene ether-co-imidazole)s as toughness modifiers for epoxy resins

A toughened epoxy was prepared by reacting an epoxy resin with a poly(arylene ether-co-imidazole)s (PAEI). The epoxy resin comprises N,N,N',N'tetraglycidyl-4,4'- methylenebisbenzenamine and 4-aminophenyl sulfone. The PAEI was prepared by reacting an aromatic bisphenol, a bisphenol imidazole, and an activated aromatic dihalide or dinitro compound in the presence of potassium carbonate in a polar aprotic solvent at an elevated temperature. The epoxies which were modified with these particular PAEI's showed a significant increase in toughness with only a 10 weight percent loading of the PAEI into the epoxy. These toughened epoxies were used to prepare composites and molded parts.

Mcdaniel, Patricia D.

Physical aging of linear and network epoxy resins

Network and linear epoxy resins principally based on the diglycidyl ether of bisphenol-A and its oligomers are prepared and studied using diamine and anhydride crosslinking agents. Rubber modified epoxies and a carbon fiber reinforced composite are also investigated. All materials display time-dependent changes when stored at temperatures below the glass transition temperature after quenching (sub-T/g/ annealing). Solvent sorption experiments initiated after different sub-T(g) annealing times demonstrate that the rate of solvent uptake can be indirectly related to the free volume of the epoxy resins. Residual thermal stresses and water are found to have little effect on the physical aging process, which affects the sub-T(g) properties of uniaxial carbon fiber reinforced epoxy material. Finally, the importance of the recovery phenomenon which affects the durability of epoxy glasses is considered.

Kong, E. S.-W.

Effects of Hygrothermal Cycling on the Chemical, Thermal, and Mechanical Properties of 862/W Epoxy Resin

The hygrothermal aging characteristics of an epoxy resin were characterized over 1 year, which included 908 temperature and humidity cycles. The epoxy resin quickly showed evidence of aging through color change and increased brittleness. The influence of aging on the material s glass transition temperature (Tg) was evaluated by Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA). The Tg remained relatively constant throughout the year long cyclic aging profile. The chemical composition was monitored by Fourier Transform Infrared Spectroscopy (FTIR) where evidence of chemical aging and advancement of cure was noted. The tensile strength of the resin was tested as it aged. This property was severely affected by the aging process in the form of reduced ductility and embrittlement. Detailed chemical evaluation suggests many aging mechanisms are taking place during exposure to hygrothermal conditions. This paper details the influence of processes such as: advancement of cure, chemical degradation, and physical aging on the chemical and physical properties of the epoxy resin.

Miller, Sandi G.

Cobalt Ions Improve the Strength of Epoxy Resins

Technique developed for improving mechanical strength of epoxy resins by adding cobalt ions in form of tris(acetylacetonato)cobalt (III) complex. Solid cast disks prepared from cobalt ion-containing epoxy resins tested for flexural strength and stiffness. Incorporation of cobalt ions into epoxies increased flexural strength of resins by 10 to 95 percent. Suitable resins for this technique include any liquid or solid TGMDA resins. Improved epoxy formulation proves useful as composite matrix resin, adhesive, or casting resin for applications on commercial and advanced aircraft.

Stoakley, D. M.

Synthesis and characterization of bisimide amines and bisimide amine-cured epoxy resins

A study has been conducted with the objective of developing tough, moisture resistant, high char yield epoxy resins using novel bisimide amine (BIA) hardeners as curing agents with MY-720, a commercial state-of-the-art epoxy resin system. BIA cured epoxies are shown to have lower moisture absorption than MY-720 and other state-of-the-art epoxy resins; the tensile strengths and strain-to-failures of several of the bisimide epoxy resins (IME's) are higher than those of the state-of-the-art epoxies. Most IME's have compression properties equivalent to those of state-of-the-art epoxies. Two resin systems, IME-10 and IME-12-3, have better overall properties than other resin systems investigated.

Scola, D. A.

Properties of Two Carbon Composite Materials Using LTM25 Epoxy Resin

In this report, the properties of two carbon-epoxy prepreg materials are presented. The epoxy resin used in these two materials can yield lower manufacturing costs due to its low initial cure temperature, and the capability of being cured using vacuum pressure only. The two materials selected for this study are MR50/LTM25, and CFS003/LTM25 with Amoco T300 fiber; both prepregs are manufactured by The Advanced Composites Group. MR50/LTM25 is a unidirectional prepreg tape using Mitsubishi MR50 carbon fiber impregnated with LTM25 epoxy resin. CRS003/LTM25 is a 2 by 2 twill fabric using Amoco T300 fiber and impregnated with LTM25 epoxy resin. Among the properties presented in this report are strength, stiffness, bolt bearing, and damage tolerance. Many of these properties were obtained at three environmental conditions: cold temperature/dry (CTD), room temperature/dry (RTD), and elevated temperature/wet (ETW). A few properties were obtained at room temperature/wet (RTW), and elevated temperature/dry (ETD). The cold and elevated temperatures used for testing were -125 F and 180 F, respectively. In addition, several properties related to processing are presented.

Cruz, Juan R.

Quantitation of buried contamination by use of solvents. Part 1: Solvent degradation of amine cured epoxy resins

The solubility and/or swelling of cured epoxy resins was studied using the solubility parameter method. Determination of solubility parameters were found in order to select solvents for solvent-assisted degradation of cured epoxy polymers used in spacecraft. A method for improving recovery of seeded spores is suggested for assay of buried contaminants. Three commercial epoxy resins were cured using four different alkyl amines. For each resin-amine combination, three levels of amine were used, corresponding to 1/3, 2/3, and all of the amine required to react with the oxirane groups of the resin. The solubility parameters of the 36 resulting model compounds were determined in poorly and moderately hydrogen-bonded solvents. No strongly hydrogen-bonded solvents caused dissolution or swelling. The tolerance of cured resins is discussed in terms of polymer structure.

Rheineck, A. E.

Chromium Ions Improve Moisure Resistance of Epoxy Resins

Broad spectrum of thermosetting epoxy resins used on commercial and military aircraft, primarily as composite matrices and adhesives. In new technique, chromium-ion containing epoxy with improved resistance to moisture produced where chromium ions believed to prevent absorption of water molecules by coordinating themselves to hydroxyl groups on epoxy chain. Anticipated that improved epoxy formulation useful as composite matrix resin, adhesive, or casting resin for applications on commercial and advanced aircraft. Improvement made without sacrifice in mechanical properties of polymer.

St. Clair, A. K.

Thermal expansion and swelling of cured epoxy resin used in graphite/epoxy composite materials

The paper presents results of experiments in which the thermal expansion and swelling behavior of an epoxy resin system and two graphite/epoxy composite systems exposed to water were measured. It was found that the cured epoxy resin swells by an amount slightly less than the volume of the absorbed water and that the swelling efficiency of the water varies with the moisture content of the polymer. Additionally, the thermal expansion of cured epoxy resin that is saturated with water is observed to be more than twice that of dry resin. Results also indicate that cured resin that is saturated with 7.1% water at 95 C will rapidly increase in moisture content to 8.5% when placed in 1 C water. The mechanism for this phenomenon, termed reverse thermal effect, is described in terms of a slightly modified free-volume theory in conjunction with the theory of polar molecule interaction. Nearly identical behavior was observed in two graphite/epoxy composite systems, thus establishing that this behavior may be common to all cured epoxy resins.

Adamson, M. J.

Curing of epoxy resins with 1-DI(2-chloroethoxyphosphinyl) methyl-2,4 and -2,6-diaminobenzene

Fire resistant compositions were prepared using 1-di(2-chloroethoxy-phosphinyl)methyl-2,4- and -2,6-diaminobenzene (DCEPD) as a curing agent for typical epoxy resins such as EPON 828 (Shell), XD 7342 (Dow), and My 720 (Ciba Geigy). In addition, compositions of these three epoxy resins with common curing agents such as m-phenylenediamine (MPD) or 4,4'-diaminodiphenylsulphone (DDS) were studied to compare their reactions with those of DCEPD. The reactivity of the three curing agents toward the epoxy resins, measured by differential calorimetry (DSC), was of the order MPD DCEPD DDS. The relatively lower reactivity of DCEPD toward epoxy resins was attributed to electronic effects.

Mikroyannidis, J. A.

Curing of epoxy resins with 1-/di(2-chloroethoxyphosphinyl)methyl/-2,4- and -2,6-diaminobenzene

Fire resistant compositions were prepared using 1-di(2-chloroethoxy-phosphinyl)methyl-2,4- and -2,6-diaminobenzene (DCEPD) as a curing agent for typical epoxy resins such as EPON 828 (Shell), XD 7342 (Dow), and My 720 (Ciba Geigy). In addition, compositions of these three epoxy resins with common curing agents such as m-phenylenediamine (MPD) or 4,4'-diaminodiphenylsulphone (DDS) were studied to compare their reactions with those of DCEPD. The reactivity of the three curing agents toward the epoxy resins, measured by differential calorimetry (DSC), was of the order MPD DCEPD DDS. The relatively lower reactivity of DCEPD toward epoxy resins was attributed to electronic effects.

Mikroyannidis, J. A.

Flammability of Epoxy Resins Containing Phosphorus

As part of a program to develop fire-resistant exterior composite structures for future subsonic commercial and general aviation aircraft, flame-retardant epoxy resins are under investigation. Epoxies and their curing agents (aromatic diamines) containing phosphorus were synthesized and used to prepare epoxy formulations. Phosphorus was incorporated within the backbone of the epoxy resin and not used as an additive. The resulting cured neat epoxy formulations were characterized by thermogravimetric analysis, propane torch test, elemental analysis, microscale combustion calorimetry, and fire calorimetry. Several formulations showed excellent flame retardation with phosphorous contents as low as 1.5% by weight. The fracture toughness and compressive strength of several cured formulations showed no detrimental effect due to phosphorus content. The chemistry and properties of these new epoxy formulations are discussed.

Flammability studies

Flame Retardant Epoxy Resins

As part of a program to develop fire resistant exterior composite structures for future subsonic commercial aircraft, flame retardant epoxy resins are under investigation. Epoxies and their curing agents (aromatic diamines) containing phosphorus were synthesized and used to prepare epoxy formulations. Phosphorus was incorporated within the backbone of the epoxy resin and not used as an additive. The resulting cured epoxies were characterized by thermogravimetric analysis, propane torch test, elemental analysis and microscale combustion calorimetry. Several formulations showed excellent flame retardation with phosphorous contents as low as 1.5% by weight. The fracture toughness of plaques of several cured formulations was determined on single-edge notched bend specimens. The chemistry and properties of these new epoxy formulations are discussed.

Thompson, C. M.

Synthesis and characterization of bisimide amines and bisimide amine-cured epoxy resins

An attempt is made to develop tough, moisture resistant, high char yield epoxy resins by means of novel bisimide amine (BIA) hardener curing agents and a state-of-the-art epoxy resin system. The BIAs are isolated as mixtures containing monomer, oligomer, and polymeric species, and then characterized by elemental analysis and high pressure liquid chromatography. The bisimide amine-cured epoxies (IMEs) were characterized with respect to moisture absorption, thermal properties, and physical and mechanical properties, as well as in the role of matrices in Celion 6000/IME composites. The relative toughness characteristics of each IME formulation was measured by the 10 deg off-axis tensile test, measuring the uniaxial tensile strength, shear strength, and shear-strain-to-failure of the composite systems.

Scola, D. A.

Aminophenoxycyclotriphosphazene cured epoxy resins and the composites, laminates, adhesives and structures thereof

Aminophenoxy cyclotriphosphazenes such as hexakis (4-aminophenoxy) cyclotriphosphazene and tris (4-aminophenoxy)-tris phenoxy cyclotriphosphazene are used as curing agents for epoxy resins. These 1,2-epoxy resins are selected from di- or polyepoxide containing organic moieties of the formula (CH2-CHO-CH2) m-W-R-W- (CH2CH-CH2O)m where R is diphenyl dimethylmethane, diphenylmethane; W is a nitrogen or oxygen atom; and m is 1 when W is oxygen and 2 when W is nitrogen. The resins are cured thermally in stages at between about 110 to 135 C for between about 1 and 10 min, then at between about 175 to 185 C for between 0.5 to 10 hr and post cured at between about 215 and 235 C for between 0.1 and 2 hr. These resins are useful for making fire resistant elevated temperature stable composites, laminates, molded parts, and adhesives and structures, usually for aircraft secondary structures and for spacecraft construction.

Kumar, Devendra