Microstructure and morphology of amine-cured epoxy coatings before and after outdoor exposures—An AFM study

Atomic force microscopy (AFM) has been used to study the morphology and microstructure of an amine-cured epoxy before and after outdoor exposure. Measurements were made from samples prepared in an essentially CO₂-free, H₂O-free glove box and from samples prepared in ambient conditions. For those prepared in a CO₂-free glove box, AFM imaging was conducted on (1) an unexposed air/coating surface, (2) an unexposed coating bulk, (3) an unexposed coating/substrate interface, and (4) a field exposed air/coating surface. For samples prepared in ambient conditions, only the unexposed air/coating surface was investigated. The same regions of the exposed samples were scanned periodically by the AFM to monitor changes in the surface morphology of the coating as UV exposure progressed. Small angle neutron scattering and Fourier transform infrared spectroscopy (FTIR) studies were performed to verify the microstructure and to follow chemical changes during outdoor exposure, respectively. The results have shown that amine blushing, which occurs only under ambient conditions, had a significant effect on the surface morphology and microstructure of the epoxy. The surface morphology of the samples prepared under CO₂-free, dry conditions was generally smooth and homogeneous. However, the interface and the bulk samples clearly revealed a two-phase structure consisting of bright nodular domains and dark interstitial regions, indicating an inhomogeneous microstructure. Such heterogeneous structure of the bulk was in good agreement with results obtained by small angle neutron scattering of unexposed samples and by AFM phase imaging of the degraded sample surface. The relationship between submicrometer physical changes and molecular chemical degradation is discussed. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, October 27–29, 2004, in Chicago, IL.     

Response of the seated human body to whole-body vertical vibration: biodynamic responses to sinusoidal and random vibration

The dependence of biodynamic responses of the seated human body on the frequency, magnitude and waveform of vertical vibration has been studied in 20 males and 20 females. With sinusoidal vibration (13 frequencies from 1 to 16 Hz) at five magnitudes (0.1–1.6 ms^? 2 r.m.s.) and with random vibration (1–16 Hz) at the same magnitudes, the apparent mass of the body was similar with random and sinusoidal vibration of the same overall magnitude. With increasing magnitude of vibration, the stiffness and damping of a model fitted to the apparent mass reduced and the resonance frequency decreased (from 6.5 to 4.5 Hz). Male and female subjects had similar apparent mass (after adjusting for subject weight) and a similar principal resonance frequency with both random and sinusoidal vibration. The change in biodynamic response with increasing vibration magnitude depends on the frequency of the vibration excitation, but is similar with sinusoidal and random excitation.     

Response of the seated human body to whole-body vertical vibration: discomfort caused by sinusoidal vibration

Frequency weightings for predicting vibration discomfort assume the same frequency-dependence at all magnitudes of vibration, whereas biodynamic studies show that the frequency-dependence of the human body depends on the magnitude of vibration. This study investigated how the frequency-dependence of vibration discomfort depends on the acceleration and the force at the subject–seat interface. Using magnitude estimation, 20 males and 20 females judged their discomfort caused by sinusoidal vertical acceleration at 13 frequencies (1–16 Hz) at magnitudes from 0.1 to 4.0 ms^? 2 r.m.s. The frequency-dependence of their equivalent comfort contours depended on the magnitude of vibration, but was less dependent on the magnitude of dynamic force than the magnitude of acceleration, consistent with the biodynamic non-linearity of the body causing some of the magnitude-dependence of equivalent comfort contours. There were significant associations between the biodynamic responses and subjective responses at all frequencies in the range 1–16 Hz.

Practitioner Summary: Vertical seat vibration causes discomfort in many forms of transport. This study provides the frequency-dependence of vibration discomfort over a range of vibration magnitudes and shows how the frequency weightings in the current standards can be improved.     

Use of laser scanning confocal microscopy for characterizing changes in film thickness and local surface morphology of UV-exposed polymer coatings

Laser scanning confocal microscopy (LSCM) has been used to characterize the changes in film thickness and local surface morphology of polymer coatings during the UV degradation process. With the noninvasive feature of LSCM, one can obtain thickness information directly and nondestructively at various exposure times without destroying the specimens or deriving the thickness values from IR measurement by assuming uniform film ablation. Two acrylic polymer coatings were chosen for the study, and the physical and chemical changes of the two systems at various exposure times were measured and analyzed. Those measurable physical changes caused by UV exposure include film ablation, formation of pits and other surface defects, and increases in surface roughness. It was found in both coatings that changes in measured film thickness by LSCM were not correlated linearly to the predicted thickness loss using the changes in the CH band obtained by the Fourier Transform Infrared (FTIR) spectroscopy measurements in the later degradation stages. This result suggested it was not a uniform film ablation process during the UV degradation. At later stages, where surface deformation became severe, surface roughness and profile information using LSCM were also proven to be useful for analyzing the surface degradation process Presented at the 81st Annual Meeting of the Federation of Societies for Coatings Technology, November 13–14, 2004 in Philadelphia, PA.     

YW－1无机胶的性能及应用

叙述了ＹＷ－１无机胶的粘接强度，耐高、低温性能，耐水、油、酸、碱性能，耐老化性能等，并介绍了这种胶在机械工业方面的应用，举例说明了这种无机粘接可完全取代机械制造业中所有的过盈配合，因而能创造巨大的经济价值。     

Dis-Bond Detection and the Possibility of Interfacial Stiffness Measurement with Real-Time Impulsive Stimulated Thermal Scattering

We describe a new, real-time, noninvasive method for dis-bond (delamination) detection which is based on a technique known as impulsive stimulated thermal scattering (ISTS). We first explain the ISTS technique and compare data from polyimide films tightly bound to silicon substrates with data from unsupported polyimide films. The observed differences in the data from these two cases are readily understandable and offer an unmistakable signature for delaminations. We demonstrate ISTS dis-bond detection by locating and mapping out randomly-distributed and spatially-fine regions of delamination in a polyimide film-silicon substrate system. Finally, we present two simple physical models of the interfacial region which comprehensively describe acoustic data from the tightly-bound and the unsupported samples. With insight from simulations using these models, we suggest how ISTS might be used to determine interfacial adhesion quality and we show how ISTS sensitivity to interfacial effects can be adjusted.     

Adhesion and Hydrolytic Stability of the Interface Between High-Modulus Polyethylene Fibers and Acrylic Resins

The effects of oxyen plasma treatment on the surface chemistry of Spectra 1000® high modulus polyethylene fibers and on the mechanical properties of fiber-reinforced composites of the fibers in a Bis-GMA based acrylic resin have been studied. X-ray photoelectron spectroscopy and diffuse reflectance FTIR spectroscopy have been used to show that the majority of oxygen on the fiber surface exists mostly in the form of ether and/or epoxy linkages, with carbonyl-, carboxylic- and ester-containing compounds accounting for less than 10 percent of the total. While the untreated and plasma-treated fibers have similar chemical compositions, the surfaces of the plasma-treated fibers are more polar and the oxygen is chemically bonded instead of being merely physisorbed. The interfacial shear strength between the fibers and the acrylic resin is increased by a factor of 2.3 by the plasma treatment indicating the presence of a weak boundary layer on the surface of the untreated fibers. The hydrolytic stability of the composite interfaces was investigated for fibers sized with several Bis-GMA-based adhesives. Maximum stability was attained by sizing with Bis-GMA containing a peroxide catalyst or an amine accelerator. The flexural properties of composites utilizing plasma-treated and untreated fibers were compared in three-point bending. The ultimate bending loads for composites using treated fibers were much higher than those for composites with untreated fibers, but only a fraction of that for glass or Kevlar®-reinforced materials.     

氯化聚丙烯改性胶粘剂的合成及粘附性能研究

以甲苯为溶剂，过氧化二苯甲酰(BP0)为引发剂，通过自由基聚合，采用甲基丙烯酸羟乙酯(HEMA)和苯乙烯(St)接枝改性氯化聚丙烯(CPP)。研究了不同苯乙烯用量、不同反应温度、不同反应时间、不同引发剂用量对改性氯化聚丙烯胶粘剂粘附性能的影响，得出较佳的工艺条件为反应温度90℃，反应时问2h，原料配比m(CPP)：m(HEMA)：m(St)：m(BPO)=50：0．5：0．6：0．15。     

Experimental investigations and thermodynamic modelling of KCl–LiCl–UCl3 system

Experimental investigations and Gibbs energy modelling of KCl–LiCl–UCl₃ system employing CALPHAD method are reported. Gibbs energy modelling of the subsystems KCl–UCl₃ and LiCl–UCl₃ was carried out primarily using phase diagram data from the literature. For the Gibbs energy modelling of the KCl–LiCl subsystem, new phase boundary data corresponding to four terminal compositions $(x_{\mathrm{LiCl}}=0.03$, 0.05, 0.95 and 0.97) obtained through differential thermal analysis data along with thermochemical and phase diagram data from the literature were used. Thermal analysis was also carried out for KCl–LiCl eutectic mixture containing small amounts of UCl₃ $(x_{{\mathrm{UCl}}_3}=9.03\times {10}^{-3}$ and $1.79\times {10}^{-2}$). The liquidus temperatures for these compositions were found to be 637 K and 674 K. Electromotive force data for dilute solutions of UCl₃ in the KCl–LiCl eutectic melt, measured in the temperature range 708–833 K in the present work, were found to be in good agreement with the literature data. These data were also used as input for the Gibbs energy modelling of the KCl–LiCl–UCl₃ system. In order to improve the quality of the resulting Gibbs energy functions of the quasibinaries and the quasiternary, enthalpies of mixing of the corresponding melts estimated using an empirical correlation based on surrounded-ion model were also used as input. Finally, the generated Gibbs energy functions were used to compute phase equilibria.     

Effect of rare earth elements surface treatment on tensile properties of aramid fiber‐reinforced epoxy composites

Solutions of rare earth modifier (RES) and epoxy chloropropane (ECP) grafting modification method were used for the surface treatment of aramid fiber. Tensile properties of both the aramid/epoxy composites and single fibers were tested. The effects of RES concentration on tensile properties of aramid/epoxy composites were investigated in detail to explore an optimum amount of rare earth elements in solution for modifying aramid fiber. The fracture surface morphologies of tensile specimens were observed and analyzed with the aid of SEM. The experimental results show that rare earth treatment is superior to ECP grafting treatment in promoting interfacial adhesion between the aramid fiber and epoxy matrix. Meanwhile, the tensile strengths of single fibers were almost not affected by RES treatment. The optimum performance is obtained when the content of rare earth elements is 0.5 wt %. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 1037–1041, 2004