Internal structure of bitumen/polymer/wax ternary mixtures for warm mix asphalts

Polymer modified asphalts (PMA) and warm mix asphalts (WMA) are technologies widely adopted in the paving industry. The first one is well established, while the second one is relatively new, but rapidly growing since it guarantees economic and environmental advantages. Until now PMA and WMA have been used disjointedly, but it would be useful to combine them to keep the advantages of both. One of the adopted solutions to obtain a warm effect is the addition of waxes to the asphaltic binder. Therefore, a “warm mix polymer modified asphalt” may be potentially obtained with a ternary asphalt/polymer/wax system. However, the final warm effect and performances of the binder will depend on the interactions between the three components. A preliminary investigation was done by mixing asphalt, styrene‐butadiene‐styrene block copolymer and a wax chosen among the following three categories: paraffinic, partially oxidized and maleic anhydride functionalized. The morphological and calorimetric analyses and solubility tests allowed identifying different behaviors depending on the wax type, which may preferentially interact either with the asphalt or with the polymer, thus influencing the whole binder structure. With regard to the ternary mixes, it was found that: (i) the paraffinic wax preferentially resides in the polymer‐rich phase, and slightly enhances the asphalt‐polymer compatibility; (ii) the partially oxidized wax prefers the asphaltene‐rich phase and reduces the compatibility; (iii) it is not clear where the functionalized wax is located, but it has a considerable compatibilizing effect and strongly alters the colloidal equilibrium of the asphalt‐polymer blend. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Microsphere tensiometry to measure advancing and receding contact angles on individual particles

In this paper, a method to measure the advancing and receding contact angles on individual colloidal spheres is described. For this purpose, the microspheres were attached to atomic force microscope cantilevers. Then the distance to which the microsphere jumps into its equilibrium position at the air-liquid interface of a drop or an air bubble was measured. From these distances the contact angles were calculated. To test the method, experiments were done with silanized silica spheres (4.1 μm in diameter). From the experiments with drops, an advancing contact angle of 101 ± 4° was determined. A receding contact angle of 101 ± 2° was calculated from the jump-in distance into a bubble. Both experimental techniques gave the same contact angle. In contrast, on similarly prepared planar silica surfaces, a clear hysteresis was measured with the sessile drop method; contact angles of 104.5 ± 1° and 93.8 ± 1° were determined for the advancing and receding contact angles, respectively.     

Atomic force microscopy,X-ray diffraction,X-ray photoelectron spectroscopy and thermal studies of the new melamine fiber

This paper reports the characterization of unaged and aged melamine fibers using various characterization techniques including atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM) and thermal analysis. Since melamine fiber is a relatively new fiber, very few studies on its characterization have been made. Morphological studies of the fiber surface using SEM display die lines running along the filament surface, which are characteristics of synthetic fibers and generally occur during spinning of the molten prepolymer through the spinnerets. AFM studies show that the surface of a melamine fiber filament contains a large number of hills and valleys, which are triangular in shape. AFM roughness analysis shows that melamine fiber surface is considerably rough which may aid in adhesion of the fiber with polymeric matrices. Ageing causes an increase in the surface roughness with simultaneous increase in the crystallinity of the fiber from 19.4% to 22.6%. In XPS studies, high concentrations of carbonyl and hydroxyl groups on the filament surface have been detected. Ageing causes a reduction in the hydroxyl group concentration and an increase in the carbonyl group concentration due to surface oxidation. The reduction in the surface hydroxyl groups due to ageing has also been detected in the Fourier-Transform infrared (FT-IR) spectra of the aged fibers. Thermogravimetric (TG) studies reveal a high thermal stability of the melamine fiber even in an oxidative environment such as air.     

Rubber-brass bonding: morphology of cross-sections through the bonding layers as a possible basis for classification

The extensive literature on rubber-brass bonding provides a rather complex picture of the architecture of the bonding layers. In the present work, the morphology of cross-sections through the bonding layers perpendicular to the brass surface, seen in transmission electron microscopy (TEM), is used as a means of bonding layer classification. Previous experimental results with a simplified cure mixture (consisting of 1,4-polybutadiene, elemental sulfur, N,N-dicyclohexyl-2-benzothiazylsulfenamide, and, in some cases, zinc oxide) and brass foils are reconsidered. In nearly all cases, what we term a central layer is found. It consists of two sublayers with a different content of copper sulfides. Varying deposits of sulfides exist at the brass surface and also above the central layer in the direction of the rubber bulk. The various types of bonding layer with a different type of architecture are discussed in connection with previous results obtained by analytical electron microscopy (AEM) and bonding strength measurements.     

Epoxy Infiltration into Nanoporous Aluminum Oxide

This research uses spatially-resolved electron energy-loss spectroscopy (EELS) in a scanning transmission electron microscope (STEM) to study epoxy infiltration into a nanoporous aluminum surface oxide. Imaging by scanning electron microscopy (SEM) shows that the oxide surface of an as-anodized aluminum wire consists of columnar nanopores with diameters ranging from approximately 5 -150 nm. Anodized wires were embedded in a 100 g: 28 g mixture of DGEBA (diglycidyl ether of bisphenol-A) resin and PACM20 (bis(p-aminocyclohexyl)methane) curing agent followed by a two-step cure. Electron-transparent sections were cut by ultramicrotomy. Spatially-resolved carbon and oxygen EELS profiles from the oxide are anti-correlated indicating that oxide pore walls are separated by pore interiors containing epoxy. Spatially-resolved low-loss spectral data are transformed into a measure of apparent specimen thickness. Comparisons of such data with simulations based on experimentally derived oxide topologies indicate that the pores are fully filled.     

Synthesis of single-crystalline lanthanum hexaboride nanowires by Au catalyst

Lanthanum hexaboride (LaB₆) nanowires have been successfully fabricated by the facile catalytic reaction of lanthanum (La) powders, and gas mixture of boron trichloride (BCl₃), hydrogen and argon, where Au was used as the catalyst. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected-area electron diffraction (SAED) were used to characterize the composition, morphology and structure of the samples. Single crystal column-shape LaB₆ nanowires were obtained. It is expected that LaB₆ nanowires can provide thermionic emission, field-induced emission, and thermal field-induced emission of electrons for TEM, SEM, flat panel displays, as well as many electronic devices that require high-performance electron source.     

Designing the morphology of ceria particles by precursor complexes

Ceria-based materials are widely used as catalysts, catalyst supports and electrolytes in many industrial applications. The morphological requirements of ceria particles vary depending on their applications. Here we show that complex morphologies of ceria particles can be achieved by using precursor complexes in the spray pyrolysis (SP) method. Three precursor complexes have been investigated: the complex of cerium acetate hydrate (CeA) and cerium nitrate hydrate (CeN); CeA and cerium ammonium nitrate (CeAN); and CeN and CeAN. Our results suggest that the morphological formation mechanism is highly correlated with the factors of precursor solubilities, solvent evaporation rates and precursor melting temperatures.     

Morphology of CuO through precipitation process under 2.45 GHz microwave irradiation

The morphology of CuO powders formed by a homogeneous precipitation process from aqueous copper precursor complex was investigated. The effect of 2.45 GHz microwave irradiation appeared in the characteristic morphology of the CuO microcrystal with comparison of an ordinal synthesis process. The crystallographic orientation of CuO microcrystals in the particle was examined by HRTEM. Using microwave irradiation, it was demonstrated that the morphology of the particles was kept through the decomposition of the precursor. Also the rapid transformation of a precursor to CuO in aqueous solution under microwave irradiation condition was discussed.     

DNA Comet Giemsa Staining for Conventional Bright-Field Microscopy

This study was undertaken to evaluate the compatibility of Giemsa staining protocol with the comet assay. We showed, for the first time, that DNA comets can be visualized and analyzed using Giemsa staining. We generated DNA damage dose response curves for human peripheral blood lymphocytes exposed to X-ray radiation using the comet assay with either SybrGreen I or Giemsa stain. The dose response curves were fitted by linear regressions (R² > 0.977). The SybrGreen I results showed only ~1.2-fold higher slope coefficient (method sensitivity) compared to the Giemsa results. The unexpectedly high sensitivity of Giemsa staining for the comet assay is due to the Romanowsky-Giemsa effect, the stain photo-stability and the higher resolution of bright-field imaging compared to fluorescence imaging. Our results demonstrate that Giemsa staining can effectively be used for measuring DNA damage by the comet assay. The low cost and availability of Giemsa stain makes this method affordable for any low budget research and will facilitate new applications of the comet assay in biology and medicine.