Publications

Different pre-treatment procedures of the iron surface have been developed with the intention to alter the iron/Ppy interfacial properties. These results were correlated with the impedance response of Ppy coated iron samples in a corrosive aqueous environment.

This article studies the evolution of near‐surface morphology as a function of various thermo‐mechanical treatments along the fabrication line of rolled AA5050 aluminium alloy. Ultra‐microtomy has been used to prepare cross‐sectional thin foils for transmission electron microscopy (TEM) and proper surfaces for scanning Kelvin probe force microscopy (SKPFM) analysis. A slight increase in the Volta potential difference (between the inter‐metallics and the matrix) between the as‐cast surface and the surface obtained after the first hot‐mill pass, emphasized that the changes in surface micro‐structure, which in turn affect the corrosion and electrochemical properties of the finished product, had already occurred at that stage. The Volta potential difference during the subsequent hot‐mill pass remained relatively constant. As far as the near‐surface morphology was concerned, hot‐rolling resulted in the formation of a heavily deformed surface layer. Annealing of the hot‐rolled aluminium sheet resulted in partial re‐crystallization of the surface layer. Subsequent cold‐rolling re‐introduced deformation in the near‐surface region. Copyright © 2008 John Wiley & Sons, Ltd.

No abstract is provided for this article.

The efficient design of nanoporous materials crucially depends on understanding the mass transfer mechanism. Using micro-imaging techniques we now show that apparently identical crystals can exhibit different uptake rates. Nanoporous materials find widespread applications in our society: from drug delivery to environmentally friendly catalysis and separation technologies1,2,3,4,5,6. 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 techniques7, 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) process8, propane–propene separation9,10 and adsorptive heat transformation11.

Silane coatings are applied to metal surfaces for various purposes, e.g., to form a protective layer against corrosion or to act as a primer for subsequent coating. In this work bis-1,2-(triethoxysilyl) ethane (BTSE) was used as a precursor to deposit coatings on Al 99.99% substrates with three different techniques: dipcoating (water based solution), vacuum plasma and atmospheric plasma. Infrared reflection absorption spectroscopy (IRRAS), X-ray photoelectron spectroscopy (XPS) and field emission gun-scanning electron microscope (FE-SEM) were used to characterise the structure, composition and surface morphology of the silane coatings. The aim of this investigation is to compare the surface and bulk characteristics of the films prepared with the three different methods, in order to get information on how the BTSE molecule is modified by the deposition technique. The results show that films could be deposited by both vacuum and atmospheric plasma, besides the more traditional wet dipcoating. The layers deposited by vacuum plasma can be considered as hybrid organic–inorganic, comparable to the silane layers obtained by dipcoating. Atmospheric plasma treatment, however, leads to the formation of more inorganic films richer in Si–O bonds. XPS and FTIR measurements show the presence of Si–O–Si bonds, while Si–O–Si, Si–O–C, Si–O and Si–CH3 absorption bands are revealed by IRRAS measurements.

No abstract is provided for this article.

The influence of pH of a chromate bath on the morphological and chemical properties of a chromate conversion coating, formed on Alclad 2024-T3 aluminum alloy, has been investigated by variable angle spectroscopic ellipsometry in the visible and infra-red regions. Other techniques such as glow discharge optical emission spectroscopy, transmission and scanning electron microscopy, atomic force microscopy and Auger electron spectroscopy have been used in order to confirm and sustain the results obtained with this technique. The combination of different analytical methods showed a decrease in thickness together with changes in the morphology and chemical composition of the chromate film when the pH is increased from 1.2 to 2.4. Although the complexity of the chromate system and the pronounced roughness of commercial rolled aluminum limit the accuracy of spectroscopic ellipsometry, it is demonstrated that this technique can be usefully applied to the study of thin chromate films formed on industrially relevant aluminum products.

Hydrogen embrittlement leads to mechanical degradation of metals. Hence, hydrogen sorption/desorption properties of metals need to be characterized. An electrochemical procedure based on cyclic voltammetry (CV) and potentiostatic polarization is elaborated on plain-carbon steel. The procedure consists of first two consecutive CV cycles (pretreatment and reference CV), followed by cathodic H-charging, and subsequent CV scans to study and quantify the H-sorption/desorption. Best practice in this procedure is to perform all steps consecutively without interruption or sample manipulations between steps to avoid spontaneous H-loss. The H-related interaction with the steel is clearly identified in the CV and can be differentiated from the electrolyte contribution coming from thiourea. The study confirms the role of thiourea as H-recombination poison in alkaline solution, and also demonstrates that it contributes to the CV response. Additionally, various charging times are investigated to study the time to H-saturation, and also the scan rate during the CV procedure is varied to study time-related phenomena. Dedicated discharging experiments were included in the study to complement the CV data, giving additional insights in the H-steel interaction. Moreover, hydrogen related findings are successfully verified by using a complimentary method, i.e. hot extraction. The better understanding of the peaks in the CV and the continuous procedure result in a reliable methodology to characterize the H-sorption/desorption in steel.

The occurrence of preferential grain etching (PGE) during alkaline etching of aluminum extrusion alloys from the 6XXX series is often linked to the presence of certain impurity elements such as zinc, causing an undesired etching appearance. In the presented work, an additional culprit in this context is identified, which has not been investigated yet. A clear relation between PGE and the presence of a subsurface shear layer is identified for extruded Al 6060 alloys containing 0.02 and 0.06 wt% Zn. This shear layer can be distinguished from the bulk of the metal by its difference in crystallographic texture as visualized by electron backscatter diffraction (EBSD). For the Zn enriched alloy, the <111>//ND grains are etched away faster than grains with other orientations, resulting in the grainy appearance typical for PGE. Independent of the Zn content in the alloy, once the shear layer is removed and <111>//ND grains are practically absent on the new surface, the depths variations caused by preferential etching disappear. Instead, the surface of the alloy is attacked uniformly by the caustic etch bath.

The appearance of materials and objects is important in for example household products, furniture, cars. Industries constantly adjust their fabrication parameters in order to create materials displaying the required properties. This is very time consuming and can be optimized with optical models. In literature optical models are to simulate the reflection of surfaces, but these reflections are never linked to their visual perception. In this research we aspire to create a link between the optical models and the visual perception of the surface. Steel was chosen as a case study because of its use in a wide variety of applications where the appearance of the steel is of paramount importance. Two parts are discerned in this paper: first different degrees of roughness were introduced on the steel substrates. Secondly a transparent coating is applied on the rough surfaces. The experimental data were used to predict the reflection of the surface.

The use of conductive polymers in aluminium electrolytic capacitors prevents leakage and enlarges the temperature use range when compared with their liquid counterparts. PEDOT:PSS is an outstanding candidate due to its tunable properties, i.e., electronic conductivity (10−5 to 103 S/cm), and its high thermal stability. As a result of their synthesis, PEDOT:PSS dispersions are characterized by a low pH value, which can influence pH sensitive materials such as aluminium. However, no work to date has studied the interaction between PEDOT:PSS dispersions and aluminium oxide substrates. In this work, the interface and interaction between PEDOT:PSS and an aluminium electrode were studied for the first time via odd random phase electrochemical impedance spectroscopy and analysed post mortem by SEM and AFM characterization. PEDOT:PSS dispersions at different pH values (1.9, 4.9, 5.8) were applied in a layered manner onto a non-etched aluminium substrate with a grown oxide layer on top, which provided a model system for the analysis of the interface. The analysis showed that the acidic PEDOT:PSS dispersions attacked the aluminium substrate, forming pores on the surface, but had a positive impact on the capacitance of the aluminium oxide/PEDOT:PSS systems. On the other hand, neutral dispersions did not affect the aluminium electrode, but showed poor layer formation properties, and the electrochemical analysis displayed a dispersion of results ranging from capacitive to resistive behaviour.

To date, studies assessing the safety profile of 3D printing materials for application in cardiac ablation are sparse. Our aim is to evaluate the safety and feasibility of two biocompatible 3D printing materials, investigating their potential use for intra-procedural guides to navigate surgical cardiac arrhythmia ablation. Herein, we 3D printed various prototypes in varying thicknesses (0.8 mm–3 mm) using a resin (MED625FLX) and a thermoplastic polyurethane elastomer (TPU95A). Geometrical testing was performed to assess the material properties pre- and post-sterilization. Furthermore, we investigated the thermal propagation behavior beneath the 3D printing materials during cryo-energy and radiofrequency ablation using an in vitro wet-lab setup. Moreover, electron microscopy and Raman spectroscopy were performed on biological tissue that had been exposed to the 3D printing materials to assess microparticle release. Post-sterilization assessments revealed that MED625FLX at thicknesses of 1 mm, 2.5 mm, and 3 mm, along with TPU95A at 1 mm and 2.5 mm, maintained geometrical integrity. Thermal analysis revealed that material type, energy source, and their factorial combination with distance from the energy source significantly influenced the temperatures beneath the 3D-printed material. Electron microscopy revealed traces of nitrogen and sulfur underneath the MED625FLX prints (1 mm, 2.5 mm) after cryo-ablation exposure. The other samples were uncontaminated. While Raman spectroscopy did not detect material release, further research is warranted to better understand these findings for application in clinical settings.

Visible spectroscopic ellipsometry is applied to monitor in-situ the behaviour of metal and metal oxides in various aqueous solutions. Ellipsometry measures the change in polarisation state upon reflection on a sample and is widely used for the determination of the optical properties of surfaces and thin films. The technique has the advantage that no reference measurements are needed. The use of in-situ ellipsometry in the fields of electrochemistry and corrosion is illustrated by means of three cases. These show the possibilities to obtain film thickness, film refractive index, and the surface roughness of the metal. The first case is related to oxide films on aluminium. For the native oxide (several nm thick) on the metal the roughening of the substrate as well as the changes in oxide film thickness can be observed independently. On thicker oxides (> 100 nm), it is possible to independently determine in-situ the refractive index and thickness of the oxide, as well as the interface roughness. This was shown in a study of the effect of aggressive solution son aluminium/aluminium oxide surface. The second case concerns the electrochemical polishing process of copper. A good coincidence is achieved between the interface roughness and layer thickness from ellipsometry and the expected surface structure for the different electrochemical conditions. A last example shows the possibility of ellipsometry to study the copper corrosion in an aggressive solution. For this case, the thickness and the refractive index of the corrosion film can only be obtained in that part of the spectrum where the oxide is transparent. The degree of corrosion protection was characterised by monitoring the protective film thickness.

No abstract is provided for this article.