Annemie Adriaens

Ghent University, Gand, Flanders, Belgium

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Publications (97)323.55 Total impact

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    ABSTRACT: The synthesis and characterisation of a reference sample containing a distinct geometrical pattern of Cu2O (cuprite) is described. The sample is to be used as an assessment sample to evaluate a newly developed X-ray-excited optical luminescence (XEOL) microscope, built for non-destructive chemical imaging of metal and other surfaces. The sample was produced by heating in a reducing flame and subsequent air exposure. It was characterized both qualitatively and quantitatively using X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy in both fluorescence mode (XAS) and optical luminescence mode (XEOL-XAS), and X-ray diffraction (XRD). Results indicate the presence of a layered structure comprising a heterogeneous mixture of cuprite and tenorite (CuO) with mainly cuprite (91.4%) in the near-surface regions and larger amounts of tenorite in the top 1-3 nm. The cuprite produced via this protocol was found to provide intense optical luminescence upon X-ray bombardment, which is particularly useful during the evaluation of the microscope
    Applied Surface Science 02/2015; 332. DOI:10.1016/j.apsusc.2015.01.200 · 2.54 Impact Factor
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    ABSTRACT: This paper concerns a time lapse spectroelectrochemical study of the growth of lead dodecanoate layers on a lead substrate in an aqueous solution using cyclic voltammetry. In-situ synchrotron radiation X-ray diffraction measurements were carried out on station BM26A (DUBBLE) at the European Synchrotron Radiation Facility (ESRF) in France. The diffraction pattern images were taken using a two-dimensional Mar CCD camera. After deposition of the coating, a spectroelectrochemical study of a linear sweep voltammetry experiment using an acetic acid electrolyte, simulating ‘active’ lead corrosion, was carried out on both a bare and lead dodecanoate coated sample. The results show that the coating inhibits the formation of new lead corrosion products.
    Talanta 01/2015; 132:760-768. DOI:10.1016/j.talanta.2014.10.035 · 3.50 Impact Factor
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    ABSTRACT: Several heritage systems have been studied using state-of-the-art synchrotron techniques. The cultural heritage value of silver is documented in museum collections across the globe. However, the silver surface is not as chemically stable as that of other precious metals, and is susceptible to corrosion by atmospheric gases. It is therefore of special interest to clarify these surface reactions by using in-situ, time-lapse chemical and structural analysis in controlled ambients in order to develop strategies to reduce or even prevent the atmospheric attacks. In order to study the initial corrosion processes of silver in the presence of corrosive gases in-situ time-lapse X-ray diffraction experiments were performed on the XMaS beamline at the European Synchrotron Radiation Facility, Grenoble. Highly pure silver samples were weathered with synthetic air containing 500 ppb of both H2S and ozone, at relative humidity (RH) levels, and XRD patterns were tracked every 10 min over a total weathering time of 24h. The time-lapse Synchrotron Radiation (SR)-XRD data show that pure silver exposed to those atmospheres starts to form crystalline corrosion products after only 10 minutes. Silver sulfates, silver oxides, intermediates and mixed species are formed on the sample surface over the duration of the experiment. The data collected using a newly combined environmental cell/gas flow set up introduces a set of highly useful tools for scientists who wish to study time-lapse gaseous corrosion at ambient temperature and pressure.
    Journal of Analytical Atomic Spectrometry 01/2015; DOI:10.1039/C4JA00392F · 3.40 Impact Factor
  • Koodlur Sannegowda Lokesh, Annemie Adriaens
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    ABSTRACT: Figure: Cyclic voltammograms of GCEs in 0.5 M H2SO4 at 5 mV/s in N2: i) pristine and ii) modified with poly(PdTAPc). The polymeric palladium tetraaminephthalocyanine has been prepared by electropolymerization. The polymer is characterized and showed very good supercapacitance behavior in 0.5 M H2SO4.
    Dyes and Pigments 01/2015; 112:192–200. DOI:10.1016/j.dyepig.2014.06.034 · 3.47 Impact Factor
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    ABSTRACT: The hydrolysis of nantokite to form cuprite could be a reaction step in the progression of bronze disease on cupreous objects d'art. In this paper, this transformation is visualized for the first time using a time-resolved synchrotron X-ray diffraction experiment. Complete conversion of nantokite to cuprite was observed on a nantokite patina over 5 h in water using time-resolved synchrotron X-ray diffraction.
    Corrosion Science 11/2014; 91. DOI:10.1016/j.corsci.2014.11.021 · 3.69 Impact Factor
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    ABSTRACT: The application of a modular system for the non-destructive chemical imaging of metal and other surfaces is described using heritage metals as an example. The custom-built X-ray-excited optical luminescence (XEOL) microscope, XEOM 1, images the chemical state and short-range atomic order of the top 200 nm of both amorphous and crystalline surfaces. A broad X-ray beam is used to illuminate large areas (up to 4 mm²) of the sample, and the resulting XEOL emission is collected simultaneously for each pixel by a charge-coupled device (CCD) sensor to form an image. The input X-ray energy is incremented across a range typical for XANES and an image collected for each increment. The use of large-footprint beams combined with parallel detection allows the power density, to be kept low and facilitates complete non-destructive XANES mapping on a reasonable timescale. In this study the microscope was evaluated by imaging copper surfaces with well-defined patterns of different corrosion products (cuprite Cu2O and nantokite CuCl). The images obtained show chemical contrast, and filtering the XEOL light allowed different corrosion products to be imaged separately. Absorption spectra extracted from software selected regions of interest exhibit characteristic XANES fingerprint spectra for the compounds present. Moreover, when the X-ray absorption edge positions were extracted from each spectrum an oxidation state map of the sample could be compiled. The results show that this method allows one to obtain non-destructive and non-invasive information at the micron-scale whilst using full-field imaging.
    Analytical Chemistry 11/2014; DOI:10.1021/ac503284r · 5.83 Impact Factor
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    ABSTRACT: Objective To assess the site-specific corrosive behaviour of the frameless IUD following long-term exposure to the uterine environment. Study design A qualitative and morphological study using X-ray diffraction (XRD) and scanning electron microscopy (SEM). Results Three GyneFix® IUDs which were in site up to 150 months were examined. In utero corroded copper sleeves were divided into 10 different groups based on their shape (U or O), orientation (inside or outside) and in utero residence time. X-ray diffraction indicated the presence of solely cuprite (Cu2O) as corrosion product on both the inside and the outside of the copper sleeves, regardless of their shape. These results were confirmed by backscattered electron micrographs recorded on the inside, the outside and the cross-section of the IUD sleeve. SEM results suggest that shape and orientation slightly affect the corrosion rate. Conclusion The apparent copper loss from both sides of GyneFix copper tubes proves that both sides are a potential copper source and therefore justifies the design of GyneFix IUD. This could be beneficial for women as the IUD could be reduced in size and therefore better tolerated. The impact on bleeding could also be minimized.
    Contraception 10/2014; 90(4). DOI:10.1016/j.contraception.2014.05.009 · 3.09 Impact Factor
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    ABSTRACT: Background: Ethanolic solutions of long-chain carboxylic acids can be applied to lead metal substrates to form a coating of lead carboxylate which provides protection against atmospheric pollutants. Results and conclusions: In this paper we describe the optimal inhibitor concentration for the coating on lead. Electrochemical impedance data taken before and after immersion in media modelling oak emitted volatile organic compounds (VOCs) polluted atmospheres show that coating effectiveness decreases after exposure, but the effect is lessened if longer chain carboxylates are used.
    07/2014; 2(1):14. DOI:10.1186/2050-7445-2-14
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    ABSTRACT: This work investigates the effect of the ceria nanoparticle concentration on the morphology and electrochemical behavior of cerium-silane hybrid coatings deposited on electro-galvanized steel substrates. The substrates were pre-treated with 3-glycidoxypropyl-trimethoxysilane and bisphenol A, modified with cerium ion-activated CeO2 nanoparticles. The morphology of the coating before and after corrosion tests was examined using atomic force microscopy and scanning electron microscopy. The results indicate the formation of nanostructured surfaces with relatively uniform thicknesses and nanoparticle distribution. Microscopic observations explain the increased durability of the silane coating doped with the lowest content of activated ceria nanoparticles after short-term corrosion tests (456 h). The corrosion behavior of the sol- gel coatings was also investigated using natural salt spray tests, electrochemical impedance spectroscopy, and potentiodynamic polarization tests. The results show that the concentration of nanoparticles has a significant impact on the barrier properties of the silane films, which are improved for films with lower nanoparticle contents.
    Materials Chemistry and Physics 06/2014; 145(3):450–460. DOI:10.1016/j.matchemphys.2014.02.035 · 2.13 Impact Factor
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    ABSTRACT: We discuss the effectiveness of a lead tetradecanoate coating on lead to protect against harmful volatile organic compounds emitted from oak. The oak volatile organic compounds were characterized by GCMS and the major constituent was found to be acetic acid. Under the test conditions, the coating decreases the rate of corrosion by up to 75% compared to bare lead. The thickness of corrosion products on the sample was also calculated thus demonstrating the power of the time-lapse synchrotron radiation X-ray diffraction technique to deliver a quantitative estimate of the effectiveness of the coating. (C) 2014 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license.
    Corrosion Science 05/2014; 82:280–289. DOI:10.1016/j.corsci.2014.01.027 · 3.69 Impact Factor
  • Alice Elia, Mark Dowsett, Annemie Adriaens
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    ABSTRACT: This work presents the application of voltammetry of microparticles (VMP) to the characterization of metallic artefacts. The paper illustrates the principle of the technique and the methods for the identification of metals and copper minerals. VMP can be considered a non-invasive technique as it requires a minimum amount of material for performing the analyses. To emphasize the efficacy of this technique regarding characterization of cultural heritage materials, two bronze artefacts of different historical periods were investigated. By using a paraffin-impregnated graphite electrode, the composition of the alloy and the copper minerals present in their patinas were analysed and identified. The results obtained from the electrochemical characterization were confirmed by complementary analysis carried out with X-ray fluorescence and X-ray diffraction.
    Applied Physics A 02/2014; 118(2). DOI:10.1007/s00339-014-8342-2 · 1.69 Impact Factor
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    ABSTRACT: In order to understand the corrosive and morphological characteristics of lead dodecanoate protective coatings on real samples, three pipe organ samples were studied using optical microscopy (OM), scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), and electrochemical impedance spectroscopy (EIS). The corrosion products and elemental composition of the top layer of the different pipe organ samples were investigated. The results indicate that the three pipe organ samples are made of an alloy composed mainly of lead and tin. After immersion and the deposition of the protective coating, only lead and no tin is detected, which indicates the formation of a thick coating containing lead dodecanoate complexes.
    Applied Surface Science 02/2014; 292:149–160. DOI:10.1016/j.apsusc.2013.11.103 · 2.54 Impact Factor
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    Farzin Arjmand, annemie adriaens
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    ABSTRACT: Capillary–based microcells, also known as microcapillary electrochemical droplet cells, have proved their capabilities in various electrochemical surface investigations in recent decades. Due to the large measured current density and the high limiting current, this technique provides high– resolution electrochemical responses. Current densities in the range from a few femto to pico Acm−2 to hundreds of Acm−2 can be measured using this technique. Various applications for microcapillary cells have been reported. Technical limitations, such as the Ohmic drop and changes in the composition of the measurement area near the tip of the microcapillary have also been considered by some researchers. The rapid increase in the application of microcells and the increase in the number of related reports published in the literature have paralleled recent attempts to develop and improve microcell setups, showing that this technique is already well established for electrochemical surface studies.
    Journal of Solid State Electrochemistry 01/2014; 18(7). DOI:10.1007/s10008-014-2413-3 · 2.23 Impact Factor
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    ABSTRACT: Polarization and impedance measurements in a corrosive environment have been used to investigate the adsorption and corrosion inhibition characteristics of sodium dodecanoate on lead. Results show that the concentration of sodium dodecanoate has an important effect on the anodic lead dissolution. Monolayer adsorption occurs at low inhibitor concentrations. The equilibrium constant (Kads), calculated using the Frumkin model, is about 10−5 M−1. Multilayer formation at concentrations above the critical micelle concentration ensures the formation of a lead dodecanoate coating following the dissolution-precipitation mechanism. These lead complexes are formed on top of the surface, which has been confirmed by secondary electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS) and X-ray photoelectron spectroscopy (XPS).
    Journal of The Electrochemical Society 01/2014; 161(3):C126-C137. DOI:10.1149/2.071403jes · 2.86 Impact Factor
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    ABSTRACT: In experiments preliminary to the design of an x-ray excited optical luminescence (XEOL) based chemical mapping tool we have used x-ray micro (4.5 μm × 5.2 μm) and macro (1 mm × 6 mm) beams with similar total fluxes to assess the effects of a high flux density beam of x-rays at energies close to an absorption edge on inorganic surfaces in air. The near surface composition of corroded cupreous alloys was analysed using parallel x-ray and optical photoemission channels to collect x-ray absorption near-edge structure (XANES) data at the Cu-K edge. The x-ray fluorescence channel is characteristic of the composition averages over several microns into the surface, whereas the optical channel is surface specific to about 200 nm. Whilst the x-ray fluorescence data were mostly insensitive to the x-ray dose, the XEOL-XANES data from the micro beam showed significant dose-dependent changes to the superficial region including surface cleaning, changes in the oxidation state of the copper, and destruction of surface compounds responsible for pre-edge fluorescence or phosphorescence in the visible. In one case there was evidence that the lead phase in a bronze had melted. Conversely, data from the macro-beam were stable over several hours. Apart from localized heating effects, the micro-beam damage is probably associated with the O3 loading of the surface and increased reaction rate with atmospheric water vapour.
    Analytical Chemistry 09/2013; 85(20). DOI:10.1021/ac401646q · 5.83 Impact Factor
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    Wenjuan Liu, Farzin Arjmand, Fehe Cao, Annemie Adriaens
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    ABSTRACT: We report the use of voltammetry of immobilized microparticles for the quantification of metallic copper and nickel in their binary mixtures. Twenty-two electrolytes were investigated in order to obtain well-separated oxidation peaks. An experimental design strategy was employed to study the effect of the electrolyte concentration and the scan rate on the resolution of the oxidation peaks. With the optimum experimental parameters, a quantification was performed and the linear results of percentage of anodic currents in term of their relative amount in the binary mixture were obtained. Finally, the prediction of two mixture samples was performed and gave satisfactory results.
    International journal of electrochemical science 02/2013; 8:2576 - 2585. · 1.96 Impact Factor
  • Roohangiz Zandi Zand, Kim Verbeken, Annemie Adriaens
    International journal of electrochemical science 01/2013; 8(1):548-563. · 1.96 Impact Factor
  • Roohangiz Zandi Zand, Kim Verbeken, Annemie Adriaens
    International journal of electrochemical science 01/2013; 8(4):4924-4940. · 1.96 Impact Factor