Publications

Many papers dealing with the surface analysis of plasma polymers or plasma‐modified polymers report the use of X‐ray photoelectron spectroscopy (XPS) to quantify the surface composition. However, most of the time, quantification is performed using software that includes an equation based on the assumption that the sample is homogeneous in composition. However, for plasma‐treated samples, this is often not the case. The usual analysis of XPS spectra does not allow the exact quantification in the case of an inhomogeneous sample. In this paper, we show that it is possible to obtain a depth profile of the composition, and a more accurate surface composition by using another mathematical approach for surface quantification, being QUASES Tougaard.

Shaping metal-organic frameworks (MOFs) into robust particles with a controllable size is of large interest to the field of adsorption. Therefore, a method is presented here to produce robust MOF beads of different sizes, ranging from 250 μm to several millimeters, which, moreover, preserve the adsorption properties of the unformulated MOF. A simple, mild, and flexible method is demonstrated with the zeolitic imidazolate framework-8 (ZIF-8)/polyvinyl formal composite material. The properties of the composite material are determined via optical imaging, scanning electron microscopy, energy-dispersive X-ray spectroscopy, inductively coupled plasma mass spectrometry, X-ray diffraction, mercury intrusion, argon porosimetry and pycnometry as well as thermogravimetric analysis/differential scanning calorimetry, crush strength tests, and immersion experiments. The proposed method allows the production of resistant particles with a high MOF loading (up to 85 wt %) and remarkable structural and textural properties required for adsorptive separation processes, including a preserved ZIF-8 crystalline structure, microporosity, and a narrow macropore size distribution (1.27 μm average). The particles show a spherical shape with an average aspect ratio of 0.85. The stability tests demonstrated that the composite MOF material exhibits a high mechanical strength (3.09 N/Pc crushing strength) almost equivalent to that of a widely used commercial zeolite material. Furthermore, the material remains stable up to 200 °C and in most solvents. The adsorption properties are explored via static and dynamic experiments in the vapor and liquid phases. The results show that the adsorption capacities are only reduced in proportion to the binder content compared with the pristine material, indicating no binder intrusion in the ZIF-8 pores. Fixed-bed experiments demonstrate the remarkable separation performance in the vapor phase, whereas mass transfer limitations arise in the liquid phase with increasing flow rate. The mass transfer limitations are attributed to the diffusion in the macropores or through the ZIF-8 crystal outer layer.

In this study, the quantification of decarburization induced during the annealing process for the fabrication of electrical steels was carried out using glow discharge optical emission spectroscopy (GD‐OES). Different calibration methods, based on external and internal standard references, were examined to optimize the quantification of carbon concentration. Accurate calibration curves for carbon at low concentration ranges were achieved by the use of carbon intensity calibrated by the internal reference, i.e. iron intensity line. This methodology was found to be beneficial for long GD‐OES measurements, providing a better correction over changes in the overall emission intensity with the sputter time. The good depth resolution obtained by the GD‐OES technique enabled the identification of specific features in the steel microstructure related to carbide coarseness. Quantitative carbon concentration profiles were obtained by GD‐OES to evaluate the decarburization effect on the microstructure of low‐carbon steels considering different initial microstructures. The effect of the spatial distribution of carbides in these microstructures on the decarburization kinetics was also studied. Through quantitative determination of carbon elemental profiles by GD‐OES, information about the morphology of the cementite in the microstructure and its development in relation to decarburization was acquired. The depth of decarburization can accurately be determined. On the basis of the global results, GD‐OES thus emerged as being a fast and reliable technique for a better understanding of decarburization kinetics. Copyright © 2015 John Wiley & Sons, Ltd.

We report on the ability to change the layer properties of porous layered radially elongated pillar (PLREP) array columns and its relevance to the separation efficiency. The adjustment of the preparation condition resulted in the formation of a 1.2-fold thicker layer than the layer produced in the preceding study. The mesoporosity of the layer was controlled by changing the hydrothermal treatment temperature from 105 °C to 80 °C. Chromatographic characterization was performed on a commercial nano-LC system using the octadecylsilylated PLREP columns having the aforementioned characteristics, i.e. (1) different layer thickness (d f = 180–220 nm) and (2) different mesoporosity (d p = 7.6–11.2 nm, Pore volume (V p) = 0.733‒0.838 cc/g and Surface area (SA) = 364‒611 m2/g). For isocratic separations of an alkylphenone mixture, the change in both the layer thickness and the mesoporosity caused no significant difference in the column efficiency, while the thicker layer and the reduction of mesopore size resulted in a 1.3-fold increase and a 1.4-fold increase in the retention capacity, respectively. Based on the result of the examination using scanning electron microscopy and argon physisorption technique, the formar enhancement was in agreement with the increase in the layer thickness, and the latter one was attributed to the larger surface area. When applying a column with 16.5 cm long to gradient separations, the combination of the thicker layer and the smaller mesopores provided the peak capacity of 365 for the alkylphenone mixture at a 180 min gradient, while the combination of the thinner layer and the larger mesopores provided the peak capacity of 315. For peptide separations, it appeared that the thicker layer was still favorable, however, the lager mesopores were more advantageous for MWs of larger than 1000, providing a conditional peak capacity of 245 for a commercially available peptide mixture because of less content of small pores which hinder the diffusion of large molecules in pores in the layer.

Sr is known to transform the morphology of the eutectic silicon phase as well as the Fe-rich β phase in Al-Si alloys, improving their mechanical properties. However, little is known about the effect Sr has on the (local) corrosion properties of aluminium alloys. This study investigates the effect of Sr addition to a modified AA3003 heat exchanger material on the morphology of the different phases present, especially the Fe-rich phases, as well as on the (local) corrosion properties of this material. This work reports the formation of a Sr-rich phase, which slightly increases the macrohardness of the material. The Fe-rich phases are not shown to be refined/influenced by the addition of Sr Potentiodynamic polarization experiments showed an increase in pitting potential by increasing the amount of Sr in the material up to 0.4 wt.%. Nevertheless, the analysis of the corrosion morphology revealed that the Sr-containing particles did not contribute to the corrosion process despite their cathodic behaviour compared to the Al matrix as measured by Scanning Kelvin Probe Force Microscopy. This behaviour was attributed to the thicker oxide layer found on the Sr-rich particles.

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No abstract is provided for this article.

The formation of corrosion product at the cut edge of aluminum-rich metal-coated steel is reported in the present work. Painted metal-coated steel samples with different amounts of Al in the metal coating, were immersed in a 0.05 M NaCl solution. The ex situ analysis of the corrosion products formed was carried out by scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDX), Raman and Fourier transform infrared (FT-IR) spectroscopy. The role of these products is discussed along with the influence of Al content in the metal coating.

No abstract is provided for this article.

Porous anodized aluminum oxides were silicate-treated by dipping in a water-based sodium silicate solution. The surface modifications occurring on the oxide layer during immersion in solution are studied as a function of the SiO2/Na2O ratio and the temperature of the silicate solution. The anionic speciation in the silicate solution was studied by means of 29Si NMR. The reactions happening at the anodic alumina surface were studied by monitoring the open circuit potential as a function of time. The presence of silicate in the pores of the anodic layer is analyzed by means of GDOES and the morphological changes occurring on the oxide surface during immersion are observed by FE-SEM. The mechanism of the deposition is extended to silicate solutions with SiO2/Na2O=1.

No abstract is provided for this article.