Isabelle Vandendael

The role of crystal diversity in understanding mass transfer in nanoporous materials

Nanoporous materials find widespread applications in our society: from drug delivery to environmentally friendly catalysis and separation technologies. The efficient design of these processes depends crucially on understanding the mass transfer mechanism. This is conventionally determined by uptake or release experiments, carried out with assemblages of nanoporous crystals, assuming all crystals to be identical. Using micro-imaging techniques, we now show that even apparently identical crystals (that is, crystals of similar size and shape) from the same batch may exhibit very different uptake rates. The relative contribution of the surface resistance to the overall transport resistance varied with both the crystal and the guest molecule. As a consequence of this crystal diversity, the conventional approach may not distinguish correctly between the different mass transfer mechanisms. Detection of this diversity adds an important new piece of evidence in the search for the origin of the surface barrier phenomenon. Our investigations were carried out with the zeolite SAPO-34, a key material in the methanol-to-olefins (MTO) process, propane-propene separation and adsorptive heat transformation.

Detailed characterization of the kinetic performance of first and second generation silica monolithic columns for reversed-phase chromatography separations

The kinetic performance of commercially available first generation and prototype second generation silica monoliths has been investigated for 2.0mm and 3.0-3.2mm inner diameter columns. It is demonstrated that the altered sol-gel process employed for the production of second generation monoliths results in structures with a smaller characteristic size leading to an improved peak shape and higher efficiencies. The permeability of the columns however, decreases significantly due to the smaller throughpore and skeleton sizes. Scanning electron microscopy pictures suggest the first generation monoliths have cylindrical skeleton branches, whereas the second generation monoliths rather have skeleton branches that resemble a single chain of spherical globules. Using recently established correlations for the flow resistance of cylindrical and globule chain type monolithic structures, it is demonstrated that the higher flow resistance of the second generation monoliths can be entirely attributed to their smaller skeleton sizes, which is also evident from the external porosity that is largely the same for both monolith generations (ɛe∼0.65). The recorded van Deemter plots show a clear improvement in efficiency for the second generation monoliths (minimal plate heights of 13.6-14.1μm for the first and 6.5-8.2μm for the second generation, when assessing the plate count using the Foley-Dorsey method). The corresponding kinetic plots, however, indicate that the much reduced permeability of the second generation monoliths results in kinetic performances (time needed to achieve a given efficiency) which are only better than those of the first generation for plate counts up to N∼45,000. For more complex samples (N≥50,000), the first generation monoliths can intrinsically still provide faster analysis due to their high permeability. It is also demonstrated that - despite the improved efficiency of the second generation monoliths in the practical range of separations (N=10,000-50,000) - these columns can still not compete with state-of-the-art core-shell particle columns when all columns are evaluated at their own maximum operating pressure (200bar for the monolithic columns, 600bar for core-shell columns). It is suggested that monolithic columns will only become competitive with these high efficiency particle columns when further improvements to their production process are made and their pressure resistance is raised.

Fatigue of Ti6Al4V Structural Health Monitoring Systems Produced by Selective Laser Melting

Selective laser melting (SLM) is an additive manufacturing (AM) process which is used for producing metallic components. Currently, the integrity of components produced by SLM is in need of improvement due to residual stresses and unknown fracture behavior. Titanium alloys produced by AM are capable candidates for applications in aerospace and industrial fields due to their fracture resistance, fatigue behavior and corrosion resistance. On the other hand, structural health monitoring (SHM) system technologies are promising and requested from the industry. SHM systems can monitor the integrity of a structure and during the last decades the research has primarily been influenced by bionic engineering. In that aspect a new philosophy for SHM has been developed: the so-called effective structural health monitoring (eSHM) system. The current system uses the design freedom provided by AM. The working principle of the system is based on crack detection by means of a network of capillaries that are integrated in a structure. The main objective of this research is to evaluate the functionality of Ti6Al4V produced by the SLM process in the novel SHM system and to confirm that the eSHM system can successfully detect cracks in SLM components. In this study four-point bending fatigue tests on Ti6Al4V SLM specimens with an integrated SHM system were conducted. Fractographic analysis was performed after the final failure, while finite element simulations were used in order to determine the stress distribution in the capillary region and on the component. It was proven that the SHM system does not influence the crack initiation behavior during fatigue. The results highlight the effectiveness of the eSHM on SLM components, which can potentially be used by industrial and aerospace applications.

Colorando Auro: third century colouring surface treatment of fire gildings

Abstract A few decades ago, heritage scientists and art historians started to study the ancient surface colouring techniques of metal art pieces. Colouring of copper and silver has already been broadly studied but no works on gold have been reported yet. This knowledge can be very important for art and technology history, conservation–restoration and surface sciences. This paper contributes to the investigation of the oldest recipe known so far to colour fire gildings. The chosen model samples, the mixture and the application of the recipe have been summarised by referring to the ancient writings known as the Arab and Syrian Alchemist Collection of M. Berthelot. The main aim of this research is to study the colour change obtained by applying the above mentioned recipe, and to identify the processes involved during this colour change. Digital imaging and scanning electron microscopy in combination with colorimetric measurements and elemental analysis have been performed to characterise the colour change and to identify its origins.

De Colorando Auro: Experiments and literature study of medieval colouring recipes on gilded plates

In the restoration-conservation practice of medieval art masterpieces, such as the Holy Lady Shrine from Huy, knowledge about the techniques used to create and shape them is of major importance, especially when they concern the surface finishing treatments. This influences the selection of methods employed for the conservation-restoration process. This paper discusses the method and the materials that might have been employed to modify the colour of gilding on silver. Recipes for chemically modifying the colour of the gilded surface can be found in medieval texts and might have been used on the masterpiece discussed in this paper. This article gives an overview of technical instructions related to this topic and presents a method to interpret their contents in order to be able to implement them. It reports observations carried out during the implementation tests, such as information about the temperature, timing, and other important elements. It concludes with the visual and the colorimetric results on the samples after application of the tested recipes.

TEM and AES investigations of the natural surface nano-oxide layer of an AISI 316L stainless steel microfibre

The chemical composition, nanostructure and electronic structure of nanosized oxide scales naturally formed on the surface of AISI 316L stainless steel microfibres used for strengthening of composite materials have been characterised using a combination of scanning and transmission electron microscopy with energy‐dispersive X‐ray, electron energy loss and Auger spectroscopy. The analysis reveals the presence of three sublayers within the total surface oxide scale of 5.0–6.7 nm thick: an outer oxide layer rich in a mixture of FeO.Fe2O3, an intermediate layer rich in Cr2O3 with a mixture of FeO.Fe2O3 and an inner oxide layer rich in nickel.

Evaluation of Different Topologies of Integrated Capillaries in Effective Structural Health Monitoring System Produced by 3D Printing

Over the last years the structural health monitoring (SHM) systems investigations have been focused on providing structures with similar functionality as the biological nervous system. There are numerous studies that have investigated this. In those studies a large number of sensors collects an extensive amount of data. In this study we demonstrate a novel effective SHM (eSHM) system which can monitor a structure with one single pressure sensor. The eSHM system can detect cracks by means of a system of capillaries integrated in a structure. This structure with the integrated capillaries can be produced by 3D printing, also known as additive manufacturing (AM). The principle of the eSHM system is monitoring the pressure variations in a network of capillaries. The effectiveness of this system is linked with the greatest strength of AM, which is the capability to create complex geometrical structures. Before the implementation in real structures, it is of crucial importance to be sure that the capillaries do not negatively influence the fatigue behaviour of the structures and the crack initiation. For this, the main objective of this study is to investigate different locations for a straight capillary incorporated into a four-point bending test specimen. The investigated titanium specimens with the integrated eSHM system are produced by AM. The capillary is located in the longitudinal dimension of the test specimen on the tension area of a four-point bending setup. We evaluate three different distances of the capillary to the outer surface of the test specimens. Furthermore, the results are also obtained by finite element simulations. We can conclude that –for the considered structure– the presence of the capillary does not influence the fatigue life negatively. On the other hand, cracks nucleate in the capillary region. Our future work will focus on the improvement of the capillary’s robustness. Other parameters like roughness effect and residual stresses should be also taken into account. doi: 10.12783/SHM2015/22