Improvement of Interfacial Adhesion of Glass Fiber/Epoxy Composite by Using Plasma Polymerized Glass Fibers

This study intends to produce plasma polymer thin films of γ-glycidoxypropyltrimethoxysilane (γ-GPS) on glass fibers in order to improve interfacial adhesion of glass fiber-reinforced epoxy composites. A low frequency (LF) plasma generator was used for the plasma polymerization of γ-GPS on the surface of glass fibers at different plasma powers and exposure times. X-ray photoelectron spectroscopy (XPS) and SEM analyses of plasma polymerized glass fibers were conducted to obtain some information about surface properties of glass fibers. Interlaminar shear strength (ILSS) values and interfacial shear strength (IFSS) of composites reinforced with plasma polymerized glass fiber were evaluated. The ILSS and IFSS values of non-plasma polymerized glass fiber-reinforced epoxy composite were increased 110 and 53%, respectively, after plasma polymerization of γ-GPS at a plasma power of 60 W for 30 min. The improvement of interfacial adhesion was also confirmed by SEM observations of fractured surface of the composites.     

Dissolution,Transport and Reaction at a DICY/DGEBA Interface

The curing of an epoxy consisting of the solid hardener dicyandiamide (DICY) and the resin diglycidyl ether of bisphenol A (DGEBA) is studied in a system consisting of a tablet of DICY embedded in liquid DGEBA. Dissolution of DICY within the liquid DGEBA in combination with the transport of dissolved DICY from the tablet border into DGEBA and the chemical reaction of both reactants is studied by scanning Brillouin microscopy and infrared spectroscopy. Scanning Brillouin microscopy demonstrates the spatial and temporal evolution of the static and dynamic hypersonic properties in the course of curing in the vicinity of the DICY tablet. Infrared spectroscopy performed on epoxy pieces extracted from the final sample at different distances from the tablet surface give information about the spatial evolution of the curing process. The results achieved by both techniques are finally combined to yield a better understanding of the curing of DICY-based epoxies, which transform upon curing from strongly heterogeneous systems towards increasingly homogeneous systems.     

Surface-Induced Interphases During Curing Processes Between Bi- and Pentafunctional Components: Reactive Coarse-Grained Molecular Dynamics Simulations

The present reactive molecular dynamics (RMD) simulations discuss the formation of interphase regions in cured polymer adhesives. The latter are obtained from the curing of reactive liquid mixtures composed of pentafunctional linkers and bifunctional monomers in contact with idealized surfaces. The present reactive scheme mimics the one of epoxies with amine linkers, i.e., processes investigated experimentally by Possart and co-workers. Generic RMD simulations are performed in a coarse-grained (CG) resolution to evaluate basic principles in curing characterized by preferential interactions. The creation of linker-rich domains is promoted by preferential surface-linker as well as linker-linker interactions in the reactive mixtures. The dimension of the interphase both in the starting mixture and the cured network depends on these preferential interactions which lead to a retardation of the curing velocity. This retardation behavior is mapped by conversion curves as a function of the number of reactive steps and by the spatially resolved profiles of the connected linkers. Although derived by generic potentials, the simulated reduction of the curing velocity is in agreement with experimental results in epoxies. The chosen interactions also imply a smaller number of linker bonds in the interphase than in the bulk region. The present RMD approach offers insight into key parameters of curing processes under the influence of preferential surface interactions coupled to selective attractions in the liquid starting mixture.     

Interfacial Chemistry of Langmuir-Blodgett Deposited Polyimide Films on Si (100)

Using the Langmuir-Blodgett (LB) technique, ultrathin films of the octadecylammonium salt of polyamic acid (PACS) on (100) oriented silicon wafers with one, three and five monolayers were prepared. The imidization of the films was investigated with x-ray photoelectron spectroscopy (XPS) during a stepwise heating procedure in vacuum. Significant differences in the XPS spectra indicate an incomplete polymerization of the films as a function of film thickness. It is believed that the chemical interaction at the interface between Si substrate and PACS is responsible for the incomplete polymerization of the LB film in direct contact with the substrate. From ellipsometric measurements the absolute thickness of a PACS and a polyimide layer has been determined to be 1.7 nm and 0.6nm, respectively. These measurements allow us to determine the electron mean free path for the Si2p electrons (E_k=1153 eV) of λ = 4.2±0.1 nm through these films.     

Deducing the Fatigue Crack Growth Rates of Natural Flaws in Silicon Nitride Ceramics: Role of R‐Curves

Fatigue failure is a concern when high‐strength, high‐toughness silicon nitride ceramics are used in mechanical components and the growth of natural flaws will determine the usable upper bound strength. In this study a fracture resistance curve (R‐curve) model is incorporated into an established method for deducing natural flaw growth rates from a combination of strength and fatigue life data for smooth specimens. Experimental data for a commercial silicon nitride, SL200, were examined. When compared with results deduced using a constant fracture toughness model, the new method gives more physically realistic growth rate results. Specifically, by incorporating the R‐curve the deduced fatigue threshold is equal to the reported intrinsic toughness for crack propagation of 2.2 MPa√m, whereas the constant fracture toughness model gives a physically unrealistic threshold value. Furthermore, much better agreement is achieved with the growth rates measured using macroscopic compact‐tension specimens. Overall, it is concluded that the R‐curve effect should not be ignored when deducing the fatigue crack growth rates of natural flaws in high‐toughness silicon nitride ceramics.     

Effect of ZnO on Crystallization of Zircon from Zirconium‐Based Glaze

The promotion of zircon (ZrSiO₄) crystallization by ZnO from a zirconium‐based frit glaze was studied and the possible mechanism was discussed. X‐ray diffraction was used to analyze the relative quantities of zircon and other transitional crystals in the samples. The results show that ZnO can significantly decrease the crystallization temperature of zirconium‐based glaze, depress the formation of Ca₂ZrSi₄O₁₂, and promote the devitrification of transitional crystals t‐ZrO₂ and Ca₂ZnSi₂O₇, as well as lead to the formation of more zircon than the ZnO‐free glaze. It was also found that zircon not only can form from the interaction between t‐ZrO₂ and SiO₂ but also can devitrify directly from the glass phase of zirconium‐based glaze.     

COMPARATIVE STUDY OF Ag2O/CO3O4 CATALYSTS PREPARED BY THE SOL-GEL AND CO-PRECIPITATION TECHNIQUES: CHARACTERIZATION AND CO ACTIVITY STUDIES

In this study effects of the preparation method on the characteristic properties and CO oxidation activities of Ag₂O/Co₃O₄ catalysts were investigated. Catalysts were prepared by two different methods: sol gel and co-precipitation. N₂ physisorption measurements, X-ray diffraction, and scanning electron microscopy measurements were used to characterize the catalysts. CO oxidation activity tests were carried out under 1% CO, 21% O₂, and the remainder He feed condition between 20° and 200°C. According to the N₂ physisorption measurements, catalysts prepared by the co-precipitation method have a higher surface area than the catalysts prepared by the sol-gel method. Co₃O₄ and AgCoO₂ phases were obtained from catalysts prepared by both techniques. In addition to these phases, metallic silver peaks were obtained by increasing calcination temperature. SEM micrographs of the catalysts showed that catalysts have uniform particles. Increasing the calcination temperature caused the formation of different-sized agglomerates and an increase in the gaps between agglomerates. The best activity was obtained from the Ag₂ O/Co₃ O₄ catalyst calcined at 200°C and prepared by the co-precipitation method. This catalyst gave 50% CO conversion at 106°C. The other two catalysts gave 100% CO conversion at a higher temperature of 200°C.     

DEVELOPMENT OF SYNERGISTIC HEAT STABILIZERS FOR PVC FROM ZINC BORATE-ZINC PHOSPHATE

The importance of flame-retardant and smoke-suppressed poly(vinyl chloride) (PVC) compositions is increasing gradually in the polymer industry since PVC releases smoke and toxic gases (hydrogen chloride, HCl) during heating at temperatures above 140°C with the result of dehydrochlorination reaction. In this study, the synergistic effects of zinc borate (ZB)-zinc phosphate (ZP) on the thermal stability of PVC were investigated using thermal techniques. The induction and stability time values of PVC plastigels were obtained at 140° and 160°C. The results revealed that PVC plastigels having only ZP and ZB retarded dehydrochlorination of PVC compared with the unstabilized sample. However, the plastigels with both ZB and ZP had a superior synergistic effect on char formation of PVC. Since the induction periods of the samples having both ZB and ZP were higher than those of the unstabilized samples having only ZB or only ZP, the synergistic effect was observed.     

HEAT AND MASS TRANSFER IN THE ADSORBENT BED OF AN ADSORPTION HEAT PUMP

The heat and mass transfer equations governing an adsorbent bed in an adsorption heat pump and the mass balance equation for the adsorbent particles in the adsorbent bed were solved numerically to simulate the cycle of a basic adsorption heat pump, which includes isobaric adsorption, isosteric heating, isobaric desorption, and isosteric cooling processes. The finite difference method was used to solve the set of governing equations, which are highly nonlinear and coupled. The pressures of the evaporator and condenser were 2 and 20 kPa, respectively, and the regeneration temperature of the bed was 403 K. Changes in the temperature, adsorptive pressure, and adsorbate concentration in the adsorbent bed at different steps of the cycle were determined. The basic simulated cycle is presented in a Clausius-Clapeyron diagram, which illustrates the changes in average pressure and temperature of the adsorbent bed throughout the cycle. The results of the simulation indicated that the most time-consuming processes in the adsorption heat pump cycle were isobaric adsorption and isobaric desorption. The high thermal resistance of the bed slows down heat transfer, prolonging adsorption and desorption processes.     

Highly efficient and versatile one-pot synthesis of substituted thienylidene compounds

A novel, efficient, and very mild one-pot synthesis of methyl 2-[(Z)-4-aryl-5-morpholino-3-oxo-2,3-dihydrothiophen-2-ylidene]acetate derivatives under kinetic control has been developed. The title compounds were prepared by the reaction of thioacetomorpholides with dimethyl acetylene-dicarboxylate (DMAD) in the presence of K₂CO₃ in a non-polar solvent with excellent yields.