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Nanocomposite films for corrosion protection
KTH, School of Chemical Science and Engineering (CHE), Chemistry, Surface and Corrosion Science.
2013 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis describes technical and scientific aspects of new types of composite films/coatings for corrosion protection of carbon steel, composite films with nanometer thickness consisting of mussel adhesive protein (Mefp1) and ceria nanoparticles, and polymeric composite coatings with micrometre thickness consisting of conducting polymer and ceria nanoparticles in a UV‐curing polyester acrylate (PEA) resin.

The influence of microstructure on corrosion behaviour was studied for a Fe‐Cr‐V‐N alloy containing micro‐sized nitrides with different chemical composition spread in martensitic alloy matrix. The Volta potential mapping suggested higher relative nobility for the nitride particles than the alloy matrix, and the nitrides with higher amounts of nitrogen and vanadium exhibited higher nobility. Potentiodynamic polarization measurements in a 0.1 M NaCl solution at neutral pH and ambient temperature showed passivity breakdown with initiation of localized corrosion which started in the boundary region surrounding the nitride particles, especially the ones enriched in Cr and Mo.

Mefp1/ceria nanocomposite films were formed on silica and metal substrates by layer‐by‐layer immersion deposition. The film formation process was studied in situ using a Quartz Crystal Microbalance with Dissipation (QCM‐D). The film grows linearly with increasing number of immersions. Increasing Mefp1 concentration or using Mefp1 with larger size leads to more Mefp1 being deposited. Peak Force Quantitative Nanomechanical Mapping (Peak Force QNM) of the composite films in air indicated that the elastic modulus of the film increased when the film deposited had a higher Mefp1 concentration. It was also noted that the nature of the outermost layer can affect bulk morphology and surface mechanical properties of the film.

The QCM‐D study of Mefp1 on an iron substrate showed that Mefp1 adsorbs at a high rate and changes its conformation with increasing adsorption time. The QCM‐D and in situ Peak Force QNM measurements showed that the addition of Fe3+ ions causes a transition in the single Mefp1 layer from an extended and soft layer to a denser and stiffer layer. In situ ATR‐FTIR and Confocal Raman Microscopy (CRM) analyses revealed complex formation between Fe3+ and catechol groups in Mefp1. Moreover, optical microscopy, SEM and AFM characterization of the Mefp1/ceria composite film formed on carbon steel showed micron‐size aggregates rich in Mefp1 and ceria, and a nanostructure of well dispersed ceria particles in the film. The CRM analysis confirmed the presence of Mefp1/Fe complexes in the film. Electrochemical impedance microscopy and potentiodynamic polarization measurements showed that the Mefp1/ceria composite film can provide corrosion protection for carbon steel, and that the protection efficiency increases with exposure time.

Composite coatings of 10 μm thickness composed of a UV‐curing PEA resin and a small amount of conductive polymer and ceria nanoparticles were coated on carbon steel. The conductive polymer (PAni) was synthesized with phosphoric acid (PA) as the dopant by chemical oxidative polymerization. The ATR‐FTIR and SEM analyses confirmed that the added particles were well dispersed in the coatings. Electrochemical measurements during long exposure in 0.1 M NaCl solution, including open circuit potential (OCP) and EIS, were performed to investigate the protective performance of the coatings. The results showed that adding ceria nanoparticles can improve the barrier properties of the coating, and adding PAni‐PA can lead to active protection of the coating. Adding PAni‐PA and ceria nanoparticles simultaneously in the coating can improve the protection and stability of the composite coating, providing excellent corrosion protection for carbon steel.

Place, publisher, year, edition, pages
Stockholm: KTH Royal Institute of Technology, 2013. , xi, 63 p.
Series
TRITA-CHE-Report, ISSN 1654-1081 ; 2013:37
Keyword [en]
corrosion protection, nanocomposite, coating, tool alloy, layer‐by‐layer, polarization, passivity, nanomechanical, topography, Mefp‐ 1, ceria nanoparticle, PAni, UV‐cure, AFM, Peak Force QNM, EIS, SEM, CRM, QCM‐D, ATR‐FTIR
National Category
Corrosion Engineering
Identifiers
URN: urn:nbn:se:kth:diva-132240ISBN: 978-91-7501-850-8 OAI: oai:DiVA.org:kth-132240DiVA: diva2:659270
Public defence
2013-11-01, Kollegiesalen, Brinellvägen 8, KTH, Stockholm, 10:00 (English)
Opponent
Supervisors
Note

QC 20131024

Available from: 2013-10-25 Created: 2013-10-24 Last updated: 2017-03-02Bibliographically approved
List of papers
1. Microstructure influence on corrosion behavior of a Fe-Cr-V-N tool alloy studied by SEM/EDS, scanning Kelvin force microscopy and electrochemical measurement
Open this publication in new window or tab >>Microstructure influence on corrosion behavior of a Fe-Cr-V-N tool alloy studied by SEM/EDS, scanning Kelvin force microscopy and electrochemical measurement
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2013 (English)In: Corrosion Science, ISSN 0010-938X, E-ISSN 1879-0496, Vol. 66, 153-159 p.Article in journal (Refereed) Published
Abstract [en]

Microstructure influence on corrosion behavior of an N-based tool alloy (Fe-Cr-V-N) has been studied. Electron microscopy analysis showed two types of hard phases in the alloy. One-pass mode scanning Kelvin force microscopy (KFM) was used to investigate relative nobility of the hard phases. Volta potential mapping indicates higher nobility for the hard phases than the alloy matrix, and, the V- and N-rich particles exhibit the highest Volta potential. Post-polarization analysis by SEM revealed localized dissolution initiated in matrix regions adjacent to hard phase particles, and the boundary region surrounding the Cr- and Mo-rich particles is more prone to localized corrosion.

Keyword
A. Alloy, B. AFM, B. Polarization, B. SEM, C. Hardening, C. Passivity
National Category
Other Chemical Engineering
Identifiers
urn:nbn:se:kth:diva-118136 (URN)10.1016/j.corsci.2012.09.013 (DOI)000313383800018 ()2-s2.0-84869502402 (Scopus ID)
Funder
Swedish Foundation for Strategic Research
Note

QC 20130213

Available from: 2013-02-13 Created: 2013-02-12 Last updated: 2017-12-06Bibliographically approved
2. Structural and Nanomechanical Properties of Paperboard Coatings Studied by Peak Force Tapping Atomic Force Microscopy
Open this publication in new window or tab >>Structural and Nanomechanical Properties of Paperboard Coatings Studied by Peak Force Tapping Atomic Force Microscopy
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2012 (English)In: ACS Applied Materials and Interfaces, ISSN 1944-8244, E-ISSN 1944-8252, Vol. 4, no 10, 5534-5541 p.Article in journal (Refereed) Published
Abstract [en]

Paper coating formulations containing starch, latex, and clay were applied to paperboard and have been investigated by scanning electron microscopy and Peak Force tapping atomic force microscopy. A special focus has been on the measurement of the variation of the surface topography and surface material properties with a nanometer scaled spatial resolution. The effects of coating composition and drying conditions were investigated. It is concluded that the air-coating interface of the coating is dominated by close-packed latex particles embedded in a starch matrix and that the spatial distribution of the different components in the coating can be identified due to their variation in material properties. Drying the coating at an elevated temperature compared to room temperature changes the surface morphology and the surface material properties due to partial film formation of latex However, it is evident that the chosen elevated drying temperature and exposure time is insufficient to ensure complete film formation of the latex which in an end application will be needed.

Keyword
atomic force microscopy, material properties, nanocomposites, coating, paperboard, topography
National Category
Chemical Sciences
Identifiers
urn:nbn:se:kth:diva-106138 (URN)10.1021/am301439k (DOI)000310109000065 ()2-s2.0-84867800986 (Scopus ID)
Note

QC 20121130

Available from: 2012-11-30 Created: 2012-11-29 Last updated: 2017-12-07Bibliographically approved
3. Nanostructured Composite Layers of Mussel Adhesive Protein and Ceria Nanoparticles
Open this publication in new window or tab >>Nanostructured Composite Layers of Mussel Adhesive Protein and Ceria Nanoparticles
2013 (English)In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 29, no 30, 9551-9561 p.Article in journal (Refereed) Published
Abstract [en]

Mussel adhesive proteins are known for their high affinity to a range of different surfaces, and they therefore appear as ideal candidates for producing thin inorganic-organic composite films with high robustness. In this work we explore the possibility of making cohesive films utilizing layer-by-layer deposition of the highly positively charged mussel adhesive protein, Mefp-1, and negatively charged ceria nanoparticles. This particular material combination was chosen due to recent findings that such films provide good corrosion protection. Quartz crystal microbalance with dissipation monitoring (QCM-D) was used for following the film formation process in situ on silica surfaces. A close to linear growth of the film with number of deposited layers was found for up to 18 deposition steps, the highest number of depositions investigated in this work. The Mefp-1 concentration during film deposition affected the film properties, where a higher protein concentration resulted in a stiffer film. It was also found that the added mass could be amplified by using a Mefp-1 solution containing small aggregates. The surface nanomechanical properties of dried multilayer films were investigated using peak force QNM (quantitative nanomechanical mapping) in air. Homogeneous surface coverage was found under all conditions explore, and the Young's modulus of the outer region of the coating increased when a higher Mefp-1 concentration was used during film deposition. The nature of the outermost surface layer was found to significantly affect the surface nanomechanical properties. The abrasion resistance of the coating was measured by using controlled-force contact mode AFM.

Keyword
Coatings, Composite films, Deposition, Elastic moduli, Film growth, Laser beam effects, Molluscs, Multilayer films, Nanoparticles
National Category
Chemical Sciences
Identifiers
urn:nbn:se:kth:diva-127764 (URN)10.1021/la401693x (DOI)000322695000030 ()2-s2.0-84881053574 (Scopus ID)
Funder
Swedish Foundation for Strategic Research Vinnova
Note

QC 20130906

Available from: 2013-09-06 Created: 2013-09-05 Last updated: 2017-12-06Bibliographically approved
4. In situ investigations of Fe3+ induced complexation of adsorbed Mefp-1 protein film on iron substrate
Open this publication in new window or tab >>In situ investigations of Fe3+ induced complexation of adsorbed Mefp-1 protein film on iron substrate
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2013 (English)In: Journal of Colloid and Interface Science, ISSN 0021-9797, E-ISSN 1095-7103, Vol. 404, 62-71 p.Article in journal (Refereed) Published
Abstract [en]

A range of in situ analytical techniques and theoretical calculations were applied to gain insights into the formation and properties of the Mefp-I film on iron substrate, as well as the protein complexation with Fe3+ ions. Adsorption kinetics of Mefp-1 and the complexation were investigated using QCM-D. The results suggest an initially fast adsorption, with the molecules oriented preferentially parallel to the surface, followed by a structural change within the film leading to molecules extending toward solution. Exposure to a diluted FeCl3 solution results in enhanced complexation within the adsorbed protein film, leading to water removal and film compaction. In situ Peak Force Tapping AFM was employed for determining morphology and nano-mechanical properties of the surface layer. The results, in agreement with the QCM-D observations, demonstrate that addition of Fe-3 induces a transition from an extended and soft protein layer to a denser and stiffer one. Further, in situ ATR-FTIR and Confocal Raman Micro-spectroscopy (CRM) techniques were utilized to monitor compositional/structural changes in the surface layer due to addition of Fe3+ ions. The spectroscopic analyses assisted by DFT calculations provide evidence for formation of tri-Fe3+/catechol complexes in the surface film, which is enhanced by Fe3+ addition.

Place, publisher, year, edition, pages
Academic Press, 2013
Keyword
Mefp-1, Complexation, QCM-D, In situ ATR-FTIR, In situ AFM, In situ confocal Raman micro-spectroscopy, DFT calculation
National Category
Chemical Sciences
Identifiers
urn:nbn:se:kth:diva-124709 (URN)10.1016/j.jcis.2013.05.016 (DOI)000320737000009 ()2-s2.0-84878984889 (Scopus ID)
Funder
Swedish Research CouncilSwedish Foundation for Strategic Research
Note

QC 20130729

Available from: 2013-07-29 Created: 2013-07-29 Last updated: 2017-12-06Bibliographically approved
5. Thin Composite Films of Mussel Adhesive Proteins and Ceria Nanoparticles on Carbon Steel for Corrosion Protection
Open this publication in new window or tab >>Thin Composite Films of Mussel Adhesive Proteins and Ceria Nanoparticles on Carbon Steel for Corrosion Protection
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2012 (English)In: Journal of the Electrochemical Society, ISSN 0013-4651, E-ISSN 1945-7111, Vol. 159, no 8, C364-C371 p.Article in journal (Refereed) Published
Abstract [en]

Thin composite films of the mussel adhesive proteins (Mefp-1) and ceria nanoparticles were deposited on substrate surfaces by alternating immersions. The film formation was studied by quartz crystal microbalance with dissipation (QCM-D) monitoring. Both the changes in frequency and dissipation recorded by QCM-D demonstrate buildup of a composite film of Mefp-1 and nanoceria. Micro-and nanostructure and composition of the film on carbon steel were characterized by optical and atomic force microscopy (AFM), electron probe micro analyzer (EPMA) and confocal Raman microspectroscopy (CRM). Optical and EPMA observations of the film show micron-sized aggregates and AFM imaging of the compact and smooth areas reveal the nanostructure. EPMA elemental mapping indicates that the micron-sized aggregates are rich in ceria and Mefp-1, whereas CRM analysis shows the presence of Mefp-1-Fe complexes in the film. Corrosion protection of the composite film on carbon steel was investigated by electrochemical impedance spectroscopy and potentiodynamic polarization measurements in NaCl solution, and compared with Mefp-1 added in the solution as an inhibitor. The measurements show that the composite film provides a higher corrosion resistance compared with Mefp-1 added as inhibitor. The corrosion resistance increases with exposure time and approaches a high level.

National Category
Corrosion Engineering
Identifiers
urn:nbn:se:kth:diva-103397 (URN)10.1149/2.061208jes (DOI)000308559400047 ()2-s2.0-85016854440 (Scopus ID)
Funder
Vinnova
Note

QC 20121011

Available from: 2012-10-11 Created: 2012-10-11 Last updated: 2017-12-07Bibliographically approved
6. The Influences of Conducting Polymer and Ceria Nanoparticles Additives on Corrosion Resistance Behavior of UV‐cure Coatings
Open this publication in new window or tab >>The Influences of Conducting Polymer and Ceria Nanoparticles Additives on Corrosion Resistance Behavior of UV‐cure Coatings
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(English)Manuscript (preprint) (Other academic)
National Category
Corrosion Engineering
Identifiers
urn:nbn:se:kth:diva-132239 (URN)
Note

QS 2013

Available from: 2013-10-24 Created: 2013-10-24 Last updated: 2013-10-25Bibliographically approved

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