Dynamic mechanical properties of three‐component composites (acrylic polymer/epoxy/SiO2) in the glass‐transition region

In previous studies, we reported the linear and nonlinear rheological properties of three‐component composites consisting of acrylic polymer (AP), epoxy resin (EP), and various SiO₂ contents (AP/EP/SiO₂) in the molten state. In this study, the dynamic mechanical properties of AP/EP/SiO₂ composites with different particle sizes (0.5 and 8 μm) were investigated in the glass‐transition region. The EP consisted of three kinds of EP components. The α relaxation due to the glass transition shifted to a higher temperature with an increase in the volume fraction (?) for the AP/EP/SiO₂ composites having a particle size of 0.5 μm, but the α relaxation scarcely shifted for the composite having a particle size of 8 μm as a general result. This result suggested that the SiO₂ nanoparticles that were 0.5 μm in size adsorbed a lot of the low‐glass‐transition‐temperature (T_g) component because of their large surface area. The AP/SiO₂ composites did not exhibit a shift in T_g; this indicated that the composite did not adsorb any component. The modulus in the glassy state (E′_g) exhibited a very weak &phis; dependence for the AP/EP/SiO₂ composites having particle sizes of 0.5 and 8 μm, although E′_g of the AP/SiO₂ composites increased with &phis;. The AP/EP/SiO₂ composites exhibited a peculiar dynamic mechanical behavior, although the AP/SiO₂ composites showed the behavior of general two‐component composites. Scanning electron microscopic observations indicated that some components in the EP were adsorbed on the surface of the SiO₂ particles. We concluded that the peculiar behavior of the AP/EP/SiO₂ composites was due to the selective adsorption of the EP component. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40409.     

Poly(p‐phenylene sulfide) nanofibers prepared by CO2 laser supersonic drawing

Poly(p‐phenylene sulfide) (PPS) nanofibers are prepared by irradiating a PPS fiber with a carbon dioxide (CO₂) laser while drawing it at supersonic speeds. A supersonic jet is generated by blowing air into a vacuum chamber through the fiber injection orifice. Nanofibers obtained at a laser power of 30 W and chamber pressure of 10 kPa exhibit an average diameter of 600 nm and a draw ratio of 110,000. Scanning electron microscopy, differential scanning calorimetry, and wide‐angle X‐ray diffraction analyses are employed to investigate the relationships among the chamber pressure, fiber morphology, and crystallization behavior. The nanofibers exhibit two melting temperatures (T_m): approximately 280°C and 320°C. The endothermic peak at T_m = 280°C is ascribable to lamellar crystals and that at T_m = 320°C to the highly complete crystals, since the polymer molecular chain is highly oriented. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40922.     

High-melt-strength polypropylene with electron beam irradiation in the presence of polyfunctional monomers

High-melt-strength polypropylene (PP) was achieved with irradiation by an electron beam generated from an accelerator in the presence of polyfunctional monomers (PFM). Among 16 PFMs, the relatively shorter molecular chain bifunctional monomers such as 1,4-butanediol diacrylate (BDDA) and 1,6-hexanediol diacrylate (HDDA) were the most effective for enhancing the melt strength of PP. The concentration and dose of the HDDA to obtain the high melt strength PP in irradiation under nitrogen gas atmosphere were 1.5 mmol/100 g PP and 1 kGy, respectively. DSC measurement and dynamic mechanical analysis showed that the thermal behavior of the high-melt-strength PP was different from that of the original PP. Crystallinity and crystallization temperature during cooling after heating were lower and higher in high melt strength PP than original PP, respectively. Elongational viscosity at 180°C of the high-melt-strength PP showed a remarkable increase at a certain elongational time with constant strain rate, demonstrating the typical property of high-melt-strength samples. This implies that a few higher molecular chains of PP, formed by intermolecular combination of its chain by HDDA in irradiation, give higher melt strength to induce entanglement of molecular chains. © 1996 John Wiley & Sons, Inc.     

Generalized warpage parameter

A warpage index (Δψ_m) was introduced for studying warpage characteristics of a plastic part injection molded from PA66 compounded with 30 wt% glass fiber. Δψ_m is defined as Δψ_m = (Δψ_m)_max – (Δψ_m)_min, where ψ_m = ψ(θ)_max, where ψ(θ) = (ε(θ) – α(θ)ΔT)/| α(θ)ΔT|, where ε is the total strain, α is the linear thermal expansion coefficient, ΔT is temperature difference, and θ is the angle along which ε and α are calculated. Finite element analysis was used for calculating flow field in injection, fiber orientation, material anisotropy and warpage. ψ_m is calculated in each finite element, and Δψ_m is calculated in a whole finite element model. Δψ_m is a measure of the ratio of actual shrinkage to the amount of shrinkage that would occur if an element freely shrank. The characteristics of Δψ_m were studied. It has been found that warpage is null if Δψ_m = 0, but that null warpage generally does not indicate Δψ_m = 0. It is shown that Δψ_m quantitatively represents the warped and unwarped state. Δψ_m distinguishes the null warpage state with possible buckling from the null warpage state without possible buckling. It has been shown that material anisotropy is possibly described with Δψ_m, and that the cause of warpage is self-restrictive deformation in an injection molded part. It has been deduced that it is generally not possible to eliminate warpage only by controlling material properties. Δψ_m is obtainable for a plastic part with complex geometry and complex fiber orientation state, and for arbitrary materials. Applications of Δψ_m are left for future study.     

Photoluminescence properties of porous silicon layers prepared by electrochemical etching in extremely dilute HF solutions

Dilute HF solutions with concentrations down to 0.03% have been used to obtain luminescent porous silicon (PSi) layers on p-type Si wafers. The experimental results show that with a constant etching time of 30 min, PSi layers with sufficient luminescence efficiencies can be formed for HF concentrations as low as 0.1%. Because of a significantly lowered critical current density, only very low etching current densities of  ≤0.1 mA cm⁻² can result in the formation of luminescent PSi samples in 0.1% HF solutions. A notable result is that these low etching current densities cannot be used to form luminescent PSi layers in concentrated ( ≥1%) HF solutions. The behavior of PL intensity as a function of etching current density has been analyzed over a wide range of HF concentration. The PL intensity is determined by the ratio of the etching current density to the critical current density, suggesting that the presence of silicon oxides plays an important role in the formation of luminescent Si nanostructures in PSi layers.     

An experimental study of flow and heat transfer of supercritical carbon dioxide in multi-port mini channels under cooling conditions

This paper presents the fluid flow and heat transfer characteristics of supercritical CO₂ in a horizontal multi-port extruded aluminum test section consisting of 10 circular channels with an inner diameter of 1.31 mm. Both local and average pressure drop and heat transfer coefficients were measured as CO₂ was cooled in the multi-port circular channels with pressures ranging from 7.4 to 8.5 MPa, inlet fluid temperatures ranging from 22 to , and mass velocity ranging from 113.7 to 418.6 kg/m² s. The results indicate that the operating pressure, the mass velocity and the temperature of CO₂ had significant effects on fluid flow and heat transfer characteristics. The pressure drop and the average heat transfer coefficient increased greatly with increasing the average temperatures of CO₂ in the near-critical region; the average heat transfer coefficient attained a peak value near the corresponding pseudocritical temperature; and the maximum heat transfer coefficient decreased as the pressure increased. Both the pressure drop and the heat transfer coefficient increased with the mass velocity, but decreased with the operating pressure. The measured average heat transfer coefficients were compared with the experimental data reported in the literatures and a large discrepancy was observed. Based on the experimental data collected in the present work, a new correlation was developed for forced convection of supercritical CO₂ in horizontal multi-port mini channels under cooling conditions.     

The result of a wall failure in-pile experiment under the EAGLE project

The WF (wall failure) test of the EAGLE program, in which 2 kg of uranium dioxide fuel-pins were melted by nuclear heating, was successfully conducted in the IGR (Impulse Graphite Reactor) of NNC/Kazakhstan. In this test, a 3 mm-thick stainless steel (SS) wall structure was placed between fuel pins and a 10 mm-thick sodium-filled channel (sodium gap). During the transient, fuel pins were heated, which led to the formation of a fuel-steel mixture pool. Under the transient nuclear heating condition, the SS wall was strongly heated by the molten pool, leading to wall failure. The time needed for fuel penetration into the sodium-filled gap was very short (less than 1 s after the pool formation). The result suggests that molten core materials formed in hypothetical LMFBR core disruptive accidents have a certain potential to destroy SS-wall boundaries early in the accident phase, thereby providing fuel escape paths from the core region. The early establishment of such fuel escape paths is regarded as a favorable characteristic in eliminating the possibility of severe re-criticality events. A preliminary interpretation on the WF test results is presented in this paper.     

Flow properties and rheology of slag from coal gasification

We have studied the rheological characteristics of Texaco gasifier slag at high-temperature. Slag samples have been analyzed by X-ray fluorescence, X-ray diffraction, and scanning electron microscopy. The rheological behavior of the slag has been investigated experimentally using a high-temperature rheometer at temperatures between 1200 °C and 1340 °C. The effects of the shear rate and temperature on the rheological behavior of the slag have been explored. Moreover, the observed rheological behavior of the slag has been correlated with its solid-phase content, as calculated with the aid of the computer software package FactSage. The results show that the sensitivity of the slag viscosity to temperature decreases with increasing rotation speed. Above its liquidus temperature calculated by FactSage, the slag behaves as a Newtonian fluid; below its liquidus temperature, however, the rheological behavior of the slag becomes non-Newtonian owing to its increased solid-phase content. Meanwhile, Slag containing a number of crystalline particles shows dramatic shear-thinning and thixotropic behavior. Moreover, the shear-thinning behavior of the slag becomes ever more distinct as the temperature is decreased. The yield stress values of the slag and the number and particle size of the crystalline particles in the slag increase with decreasing temperature.     

Kinetic arrest behavior in martensitic transformation of NiCoMnSn metamagnetic shape memory alloy

High-field magnetic measurements were carried out in order to investigate behaviors of field-induced reverse martensitic transformation and kinetic arrest of NiCoMnSn metamagnetic shape memory alloy. In the thermomagnetization curves, it was confirmed that the reverse martensitic transformation temperature decreases 67 K by applying magnetic field of 5 T, while in the magnetic field cooling process under 5 T, martensitic transformation does not occur down to low temperatures. Equilibrium magnetic field, defined from the critical magnetic fields of the metamagnetic evidence in the magnetization curves, exhibits almost constant below about 100 K, suggesting that the entropy change becomes zero, which is considered to cause kinetic arrest behavior.