Monitoring the Conservation Treatment of Corroded Cupreous Artefacts: the Use of Electrochemistry and Synchrotron Radiation Based Spectroelectrochemistry

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Monitoring the Conservation Treatment of Corroded Cupreous Artefacts: the Use of Electrochemistry and Synchrotron Radiation Based Spectroelectrochemistry FACULTY OF SCIENCE Department of Analytical Chemistry Monitoring the conservation treatment of corroded cupreous artefacts: The use of electrochemistry and synchrotron radiation based spectroelectrochemistry Thesis submitted in fulfilment of the requirements for the degree of Doctor in Science, Chemistry by Karen Leyssens Promoter: Prof. Dr. A. Adriaens Co-promoter: Dr. C. Degrigny Ghent 2006 Woord van Dank Men kan misschien wel onderzoek voeren op z’n eentj e, maar men geraakt zoveel verder met de hulp van anderen. Daarom zou ik langs deze weg graag mijn collega’s, vrienden en familie willen bedanken voor hun voortdurende steun tijdens het voltooien van dit doctoraat. Prof. Dr. A. Adriaens wens ik te bedanken voor de kans dei ze me gaf om te doctoreren, voor haar vertrouwen en de begeleiding gedurende deze 4 jaar. In het bijzonder de contacten en internationale samenwerkingen die zij tot stand bracht waren van enorme waarde voor dit werk. In this respect, I have to start with thanking Dr. C. Degrigny for suggesting several subjects of interest in the area of conservation science and even more for the discussions and support in the years thereafter. I certainly have to thank Prof. Dr. M. Dowsett from the University of Warwick for all the effort and time he invested in the design of the in situ cell and the related software, his enthusiasm during each of the measuring sessions and the hours of discussion for interpretating the XAS results. The second part of this work would not have been possible without him. Of course I should not forget all the other people involved in the synchrotron sessions for their dedication to make a succes out of each measurement. I especially want to thank Manolis Pantos for his guidance during my first sessions at the SRS and his support by processing the data, Dr. L. Vincze for the same support at the ESRF and Ingrid and Gareth for their work during and after several sessions. Bart, jij hoort meer dan wie ook thuis in dit rijtje. Elke meetsessie of congres zat je terug met mij in het team en ondanks mijn lastige bui en bleef je je goed humeur maar behouden… . Da’s echt chapeau! En ook jij, Karl, hebt je deel hier wel van gehad en toch nog beweren dat je onze treinritten gaat missen… . Ik vind jullie tweeën echt geweldig. Dank je voor al die uren die jullie voorbij deden vliegen met wetenschappelijke en persoonlijke gesprekken. En ui teraard, wanneer ik het heb over cruciale bijdragen kan ik moeilijk zwijgen over jou, Bjorn. Het was me een plezier om met jou als thesisstudent samen te werken! Ook Frederick wil ik hier nog even bedanken voor zijn inzet en inbreng bij de laatste XAS-metingen. Het bijzonder onderzoeksfonds en de Universiteit Gent ben ik zeer erkentelijk voor de financiële ondersteuning van dit doctoraatsonderzoek. Jan en Pieter, jullie wil ik ook nog even apart bedanken voor de vele uren die jullie in mijn computer/meetopstelling/werkelektrodes gestoken hebben. Naast al deze mensen die daadwerkelijk hebben bijgedragen tot het welslagen van mijn doctoraat, is er nog een caterogie die ik zeker niet mag vergeten, namelijk de groep ‘verstrooing brengers’. Hierbij wil ik alle collega’s bedanken voor de aangename werksfeer die we samen hebben opgebouwd, en waarin niet enkel wetenschappelijke maar ook menselijke aspecten aan bod konden komen. Bedankt Ine, Karolien, Brigitte, Tinne, Hans en David, voor de ontspanning tussendoor, voor de relativerende babbels op momenten van ‘hoogspanning’ of als de lettertjes en cijfertjes op mijn computerscherm, door overdosis of gewoon geen goesting, vervaagden in een ondoorgrondelijke chaos. Daarnaast wil ik natuurlijk ook vrienden en vriendinnen bedanken voor de leuke momenten samen en vooral het geduld in het zoeken naar een vrije datum hiervoor! Graag ook een bijzonder woordje van dank aan Annelies, omdat je je week achter week weer opofferde om aan mijn conditie te zwemmen en/of me mijn hart te laten luchten over allerlei (ongebelangrijke) perikelen. Je blijft een engel van een vriendin! Een heel speciale en warme dankjewel hou ik voor mijn familie. Mama en papa, heel erg bedankt voor jullie steun en vertrouwen, voor het meeleven en voor de hulp op alle vlak. Sorry voor mijn blitz-bezoekjes de laatste tijd en voor de bezorgdheid waarmee ik jullie soms opzadelde. Ruben, ook jou wil ik bedanken voor je letterlijke (figuurlijke) bijdrage aan dit werk en voor die hectische maand eind juni / begin juli dat je me gezelschap hield. En tot slot kom ik bij jou uit, Sam. Bedankt voor je waardering, je vertrouwen, je steun en je geduld. Het was goed te weten dat ik na een werkdag bij jou echt “thuis” kon komen en mezelf mocht zijn. Bedankt voor de vele momenten die we samen reeds hebben meegemaakt. Table of Contents Scope of the study ....................................................................................1 1. Copper: historical use, corrosion and conservation..............................5 1.1. General description and historical background............................................................... 5 1.2. Corrosion of copper and its alloys................................................................................... 6 1.2.1. Corrosion mechanism............................................................................................... 7 1.2.2. Corrosive environments ......................................................................................... 10 1.2.3. Typical copper corrosion compounds .................................................................... 16 1.2.4. The effect of alloying elements.............................................................................. 20 1.3. Conservation methods................................................................................................... 21 1.3.1. Storage prior to treatment....................................................................................... 22 1.3.2. Examination ........................................................................................................... 23 1.3.3. Cleaning ................................................................................................................. 23 1.3.4. Stabilization............................................................................................................ 25 1.3.4.1. Removing cuprous chloride ............................................................................ 26 1.3.4.2. Converting cuprous chloride to harmless cuprous oxide ................................ 28 1.3.4.3. Sealing cuprous chloride in the specimen from the atmosphere..................... 29 1.3.5. Storage or exhibition after cleaning ....................................................................... 29 1.4. References ..................................................................................................................... 30 2. Methods .............................................................................................37 2.1. Corrosion potential measurements................................................................................ 37 2.1.1. The corrosion potential........................................................................................... 37 2.1.2. Corrosion potential – time measurements.............................................................. 40 2.2. Other electrochemical techniques ................................................................................. 42 2.2.1. Chronoamperometry (CA) ..................................................................................... 42 2.2.2. Linear sweep voltammetry (LSW)......................................................................... 43 2.3. Synchrotron radiation based techniques........................................................................ 44 2.3.1. Synchrotron radiation (SR) .................................................................................... 44 2.3.2. X-ray diffraction (XRD)......................................................................................... 47 2.3.3. X-ray absorption spectroscopy (XAS) ................................................................... 48 2.4. Scanning electron microscopy with energy dispersive X-ray detection (SEM-EDX).. 51 2.5. References ..................................................................................................................... 53 3. Ecorr measurements of copper and copper-based alloys................57 3.1. Instrumentation.............................................................................................................. 58 3.1.1. Electrochemical cell ............................................................................................... 58 3.1.1.1. Reference electrode......................................................................................... 58 3.1.1.2. Counter electrode ............................................................................................ 59 3.1.1.3. Working electrode........................................................................................... 59 3.1.1.3.1. Materials................................................................................................... 59 3.1.1.3.2. Corrosion protocols.................................................................................. 61 3.1.1.4. Electrolyte solution ......................................................................................... 62 3.1.1.5. Instrumentation................................................................................................ 63
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