Shrinkage and internal stress during curing of epoxide resins

Shimbo, Masaki; Ochi, Mitsukazu; Shigeta, Yasuteru

doi:10.1002/app.1981.070260714

Cited by 116 publications

(46 citation statements)

References 21 publications

(1 reference statement)

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“…As a result, the volumetric shrinkage during polymerization of thermosetting resins has attracted a great deal of attention in recent years. [2][3][4][5][6] Benzoxazines are a kind of heterocyclic compounds which can polymerize via a ring-opening reaction without yielding any small molecular byproducts. It should be noted that this kind of material exhibits not only no shrinkage but also a slight expansion after curing.…”

Section: Introductionmentioning

confidence: 99%

Study on the volumetric expansion of benzoxazine curing with different catalysts

Liu

2002

J of Applied Polymer Sci

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A systematic investigation on the volumetric expansion of four benzoxazine systems, which are benzoxazine, benzoxazine/tertiary amine, benzoxazine/organic acid, and benzoxazine/epoxy resin/tertiary amine, was done. By using gravitometric and dilatometric methods, etc., studies on volumetric shrinkage, isothermal cure shrinkage, and density versus cure time plots were done. The cure reactions of these benzoxazines were carried out at 140 and 160°C. The results show that all benzoxazine systems exhibit apparent volumetric expansion after polymerization, that is, the densities of monomers are larger than are those of polymers at room temperature. But, meanwhile, they exhibit volumetric shrinkage while curing isothermally. The results also show that the higher the cure temperature is, the larger the cure shrinkage of the benzoxazines will be and that the extent of the cure shrinkage of the benzoxazines with the aid of catalysts is larger than is that of thermal polymerization systems. The reason for this is that, accelerated by catalysts, the polymerization rate become faster and the extent of polymerizatiom becomes larger. It is obvious that catalysts can make a notable impact on the cure reaction of benzoxazines. Therefore, the dimension of the volumetric expansion of benzoxazine is associated with its polymerization mechanism, molecular structure, and extent of polymerization.

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Section: Introductionmentioning

confidence: 99%

Study on the volumetric expansion of benzoxazine curing with different catalysts

Liu

2002

J of Applied Polymer Sci

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“…Therefore, at 80°C the matrix was in a rubbery state and the shear rigidity was as small as a few hundredths of that in the glassy state at room temperature (17) . For this reason, negligible shear stress arose at the fiber/matrix interface, resulting in a stress-free fiber at 80°C.…”

Section: Effect Of Heating Temperaturementioning

confidence: 99%

Dependence of Fiber Stresses on Cyclic Changes of Temperature and Water Absorption in Carbon/Epoxy Single-Fiber Model Composites

Miyake

Futamura

Fujiyoshi

et al. 2010

JMMP

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In this study, we examine the variation in residual stresses in polymer matrix composites with cyclic changes in hygrothermal environments by measuring the axial stresses in the fiber of single-carbon fiber/epoxy resin model composites using Raman microspectroscopy. To change the temperature and water absorption in the specimens separately and simultaneously, the specimens were (1) heated and cooled at atmospheric environment, (2) immersed in water and dried at room temperature, and (3) immersed in hot water (80°C) and cooled to room temperature in water and then dried. All specimens were thus restored to their initial states and then evaluated. In the cases of (1) and (2), the fiber stresses reverted to almost the same as their initial states, but in the case of (3) the axial stress after hygrothermal cyclic change was more compressive compared to the initial state. The differences among the results of the three cases are discussed based on the fiber stresses at elevated temperature, which were evaluated by Raman microspectroscopic measurement performed at temperatures ranging from room temperature to those above the glass-transition temperature of the epoxy matrix resin.

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“…A lot of studies on the curing mechanism of epoxy resin 1 and also on the residual stress 2 at the interface between metal and epoxy resin were reported, but little is known about the effects of pressure on curing behavior. It is well known that many reactions which could not be carried out under normal pressure, for example, polymerization of ethylene, can be carried out under high pressure.…”

Section: Substancesmentioning

confidence: 99%

Pressure Dependence of the Curing Behavior of Epoxy Resin

Nakamae

Nishino

Airu

et al. 1991

Polym J

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ABSTRACT:Epoxy resin of bisphenol A type/aromatic diamine system was cured under high pressure up to 1,000 MPa. Pressure dependence of the mechanical and thermal properties of cured epoxy resin was investigated. Mechanical properties such as Young's modulus, tensile strength and elongation at break, and the glass transition temperature decreased with increasing curing pressure, though high pressure showed no effect on density. The swelling ratio of the cured resin with toluene increased with increasing curing pressure, and the IR absorption band assigned to epoxy group remained for the epoxy resin cured at high pressure. These results show that high curing pressure increases the glass transition temperature, restricts the diffusion and collision of molecules and the rate of curing reaction slow down. Poor mechanical and thermal properties for the epoxy resin cured under high pressure are considered to be due to insufficient curing of these resins.KEY WORDS Ultrahigh Curing Pressure/ Epoxy Resin/ Thermal Property / Mechanical Property / Curing Behavior / substances. Epoxy resin is used in many important fields as an excellent thermosetting adhesive and protective for metals and semiconductors. A lot of studies on the curing mechanism of epoxy resin 1 and also on the residual stress 2 at the interface between metal and epoxy resin were reported, but little is known about the effects of pressure on curing behavior. It is well known that many reactions which could not be carried out under normal pressure, for example, polymerization of ethylene, can be carried out under high pressure. 3 Pressure is considered to take part in various reactions for a many In this study, epoxy resin was cured under an ultrahigh pressure up to 1000 MPa, and the pressure dependence of the mechanical and thermal properties of cured epoxy resin was investigated. EXPERIMENT AL MaterialsA liquid diglycidyl ether of bisphenol A type epoxy resin (Epikote 828; Shell Chemical Co.;

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Shrinkage and internal stress during curing of epoxide resins

Cited by 116 publications

References 21 publications

Study on the volumetric expansion of benzoxazine curing with different catalysts

Study on the volumetric expansion of benzoxazine curing with different catalysts

Dependence of Fiber Stresses on Cyclic Changes of Temperature and Water Absorption in Carbon/Epoxy Single-Fiber Model Composites

Pressure Dependence of the Curing Behavior of Epoxy Resin

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