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An in situ spectro-electrochemical study of aluminium/polymer interfaces: development of ATR-FTIR and its integration with EIS for corrosion studies
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
2006 (English)Licentiate thesis, comprehensive summary (Other scientific)
Abstract [en]

In order to extend the applications of aluminium, organic coatings may be applied on sheet materials, for instance for corrosion protection or aesthetic surface finish purposes in the automotive and construction industries, or on foil materials in the flexible packaging industry.

The most common mechanisms for deterioration and structural failure of organically coated aluminium structures are triggered by exposures to the surrounding environment. Despite the great importance to elucidate the influence of exposure parameters on a buried aluminium/polymer interface, there is still a lack of knowledge regarding the mechanisms that destabilise the structure. It is generally believed that a detailed in situ analysis of the transport of corroding species to the buried interface, or of surface processes occurring therein, is most difficult to perform at relevant climatic and real-time conditions.

In this work, Attenuated Total Reflection Fourier Transform Infrared Spectroscopy (ATR-FTIR) in the Kretschmann-ATR configuration was successfully applied to in situ studies of the transport of water and ionic species through polymer films to the aluminium/polymer interface upon exposure to ultra pure deionised water and to a 1 M sodium thiocyanate (NaSCN) model electrolyte. Other main processes distinguished were the formation of corrosion products on the aluminium surface and swelling of the surface-near polymer network. Hence, in situ ATR-FTIR was capable to separate deterioration-related processes from each other.

To perform more unambiguous interpretations, a spectro-electrochemical method was also developed for in situ studies of the buried aluminium/polymer interface by integrating the ATR-FTIR technique with a complementary acting technique, Electrical Impedance Spectroscopy (EIS). While transport of water and electrolyte through the polymer film to the aluminium/polymer interface and subsequent oxidation/corrosion of aluminium could be followed by ATR-FTIR, the protective properties of the polymer as well as of processes at the aluminium surface were simultaneously studied by EIS. The integrated set-up provided complementary information of the aluminium/polymer sample investigated, with ATR-FTIR being sensitive to the surface-near region and EIS being sensitive to the whole system. While oxidation/corrosion and delamination are difficult to distinguish by EIS, oxide formation could be confirmed by ATR-FTIR. Additionally, while delamination and polymer swelling may be difficult to separate with ATR-FTIR, EIS distinguished swelling of the polymer network and also identified ultimate failure as a result of delamination.

The capability of the integrated ATR-FTIR / EIS in situ technique was explored by studying aluminium/polymer systems of varying characteristics. Differences in water and electrolyte ingress could be monitored, as well as metal corrosion, polymer swelling and delamination.

Place, publisher, year, edition, pages
Stockholm: KTH , 2006. , viii, 38 p.
Keyword [en]
: ATR-FTIR; EIS; spectro-electrochemical; interface; aluminium; polymer
National Category
Other Chemistry Topics
Identifiers
URN: urn:nbn:se:kth:diva-4237ISBN: 91-7178-499-3 (print)OAI: oai:DiVA.org:kth-4237DiVA: diva2:11400
Presentation
2006-12-19, E3, KTH, Lindstedtsvägen 3, Stockholm, 10:00
Opponent
Supervisors
Note
QC 20101124Available from: 2006-12-15 Created: 2006-12-15 Last updated: 2010-11-24Bibliographically approved
List of papers
1. In situ ATF-FTIR studies of the aluminium/polymer interface upon exposure to water and electrolyte
Open this publication in new window or tab >>In situ ATF-FTIR studies of the aluminium/polymer interface upon exposure to water and electrolyte
2006 (English)In: Progress in organic coatings, ISSN 0300-9440, Vol. 57, no 1, 78-88 p.Article in journal (Refereed) Published
Abstract [en]

Attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) with the Kretschmann configuration was applied for in situ studies of the transport of water and ionic species through a polymer film to an aluminium/polymer interface. The time dependent intensity changes of the infrared bands of water were used to follow the transport of water to the aluminium/polymer interfacial region and a NaSCN solution was employed as model electrolyte to follow the transport and accumulation of thiocyanate ions. Apart from water sorption and ion transport, the main processes identified were corrosion/oxidation of the aluminium surface and swelling of the polymer film. The method proved to be useful for detailed in situ studies of changes at a polymer coated metal surface, such as oxidation and surface film formation on the metal. It should also be possible to study the effects of defects and pores in the polymer film on the transport properties of water and ions to the metal/polymer interface, as well as adsorption and other chemical reactions and physical interactions in the metal/polymer interfacial region.

Keyword
Aluminium, ATR-FTIR, Coating, Interface, Water uptake
National Category
Other Chemistry Topics
Identifiers
urn:nbn:se:kth:diva-6635 (URN)10.1016/j.porgcoat.2006.07.002 (DOI)000241021200010 ()2-s2.0-33748162158 (Scopus ID)
Note
QC 20101122Available from: 2006-12-15 Created: 2006-12-15 Last updated: 2010-12-02Bibliographically approved
2. A spectroelectrochemical study of metal/polymer interfaces by simultaneous in situ ATR-FTIR and EIS
Open this publication in new window or tab >>A spectroelectrochemical study of metal/polymer interfaces by simultaneous in situ ATR-FTIR and EIS
2007 (English)In: Electrochemical and solid-state letters, ISSN 1099-0062, E-ISSN 1944-8775, Vol. 10, no 4, C27-C30 p.Article in journal (Refereed) Published
Abstract [en]

Buried aluminum/polymer interfaces were studied using a spectroelectrochemical experimental setup based on simultaneous in situ attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) and electrical impedance spectroscopy (EIS). Transport of water and electrolyte through the polymer film to the aluminum/polymer interface and oxidation/corrosion of aluminum was followed by ATR-FTIR, while the impedance behavior of the system was simultaneously studied by EIS. As the ATR-FTIR technique is specific for the aluminum/polymer interfacial region while EIS takes into account alterations of both the polymer bulk and the interface, the combined setup provides complementary information of the system investigated.

Keyword
electrochemical impedance spectroscopy, organic coatings, water, metals, thiocyanate, electrolyte, films, configuration, performance, absorption
Identifiers
urn:nbn:se:kth:diva-16375 (URN)10.1149/1.2436647 (DOI)000244071400015 ()2-s2.0-33846984579 (Scopus ID)
Note
QC 20100525Available from: 2010-08-05 Created: 2010-08-05 Last updated: 2017-12-12Bibliographically approved
3. An integrated in situ ATR-FTIR and EIS study of buried metal/polymer interfaces exposed to an electrolyte solution
Open this publication in new window or tab >>An integrated in situ ATR-FTIR and EIS study of buried metal/polymer interfaces exposed to an electrolyte solution
2007 (English)In: Electrochimica Acta, ISSN 0013-4686, E-ISSN 0019-4686, Vol. 52, 5159-5171 p.Article in journal (Refereed) Published
Abstract [en]

In situ studies of buried aluminium/polymer interfaces were performed by combining Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy (ATR-FTIR) with Electrochemical Impedance Spectroscopy (EIS). The capability of this integrated analytical set-up was explored by studying the characteristics of three different aluminium/polymer systems upon exposure to a 1 M NaSCN solution. Various qualifications of the systems were distinguished and the ingress of water and electrolyte, oxidation/corrosion of aluminium, swelling of the polymer and delamination were identified. This new set of complementary acting tools provides comprehensive information of the aluminium/polymer system, with ATR-FTIR being specific for the surface-near region and EIS taking into account changes within the whole system. While oxidation/corrosion and delamination are processes difficult to distinguish by EIS, oxide formation could be confirmed by ATR-FTIR. While it may be difficult to distinguish between delamination and polymer swelling with ATR-FTIR, these processes were more easily identified with EIS.

Keyword
IMPEDANCE SPECTROSCOPY, COATED ALUMINUM, OXIDE-FILMS, PART II, WATER, EPOXY, THIOCYANATE, CORROSION, SPECTRA, CONFIGURATION
Identifiers
urn:nbn:se:kth:diva-6637 (URN)10.1016/j.electacta.2007.02.007 (DOI)000246292100004 ()
Note
QC 20101122Available from: 2006-12-15 Created: 2006-12-15 Last updated: 2010-12-02Bibliographically approved

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