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1.
Ultramicroscopy ; 197: 1-10, 2019 02.
Artículo en Inglés | MEDLINE | ID: mdl-30439555

RESUMEN

Pigment distributions have a critical role in the corrosion protection properties of organic paint coatings, but they are difficult to image in 3D over statistically significant volumes and at sufficiently high spatial resolutions required for detailed analysis. Here we report, for the first time, large volume analytical serial sectioning tomography of an organic composite coating using a xenon Plasma Focused Ion Beam (PFIB) combined with secondary electron imaging, energy dispersive X-ray (EDX) spectrum imaging (SI) and electron backscattered diffraction (EBSD). Together these techniques provide a comprehensive quantitative description of the physical orientation and distribution of the pigments within a model marine ballast tank coating, as well as their crystallographic and elemental characterisation. Polymers and organic materials are challenging because of their propensity for ion beam damage and possible beam heating effects. Our novel, optimised block preparation technique permits automated data acquisition with minimal operator intervention, and can have significant applications for the structural and chemical characterisation of a wide range of organic materials. Our results revealed that the paint contained 7.5 vol% aluminium flakes and 25 vol% quartz particles. The aluminium flakes were oriented parallel to the substrate surface, which is beneficial in terms of the corrosion protection capability of the coating.

2.
Sci Rep ; 8(1): 17450, 2018 11 28.
Artículo en Inglés | MEDLINE | ID: mdl-30487636

RESUMEN

Polyphosphate corrosion inhibitors are increasingly marketed as chromate replacements for coil coated steel. The mechanisms underpinning corrosion prevention by these species is, however, not fully understood; corrosion inhibition is ordinarily assessed using electrochemical techniques, followed by ex-situ surface analysis. As a result, the formation of a clear film over cathodic sites is known to contribute to corrosion prevention, but little is known about its formation. Here, we apply advanced microscopy techniques (in-situ fluid cell AFM, SEM-EDX, and AFM-IR nano-chemical analysis) to examine early cathodic film formation by strontium aluminium polyphosphate (SAPP) in detail. For a model cut edge system, it is found that cathodic inhibition dominates during the first 24 hours of immersion, and surprisingly, that strontium carbonate impurities play a significant role. Rapidly precipitated zinc carbonate provides protection almost immediately after immersion, before the film structure evolves to include (poly)phosphate species. This suggests that the purposeful inclusion of carbonates may provide a new, environmentally sound approach to enhancing inhibitor efficacy.

3.
ACS Appl Mater Interfaces ; 8(1): 959-66, 2016 Jan 13.
Artículo en Inglés | MEDLINE | ID: mdl-26694687

RESUMEN

The first direct observation of a chemically heterogeneous nanostructure within an epoxy resin is reported. Epoxy resins comprise the matrix component of many high performance composites, coatings and adhesives, yet the molecular network structure that underpins the performance of these industrially essential materials is not well understood. Internal nodular morphologies have repeatedly been reported for epoxy resins analyzed using SEM or AFM, yet the origin of these features remains a contentious subject, and epoxies are still commonly assumed to be chemically homogeneous. Uniquely, in this contribution we use the recently developed AFM-IR technique to eliminate previous differences in interpretation, and establish that nodule features correspond to heterogeneous network connectivity within an epoxy phenolic formulation.

4.
Faraday Discuss ; 180: 511-26, 2015.
Artículo en Inglés | MEDLINE | ID: mdl-25927079

RESUMEN

Lithium carbonate and lithium oxalate were incorporated as leachable corrosion inhibitors in model organic coatings for the protection of AA2024-T3. The coated samples were artificially damaged with a scribe. It was found that the lithium-salts are able to leach from the organic coating and form a protective layer in the scribe on AA2024-T3 under neutral salt spray conditions. The present paper shows the first observation and analysis of these corrosion protective layers, generated from lithium-salt loaded organic coatings. The scribed areas were examined by scanning and transmission electron microscopy before and after neutral salt spray exposure (ASTM-B117). The protective layers typically consist of three different layered regions, including a relatively dense layer near the alloy substrate, a porous middle layer and a flake-shaped outer layer, with lithium uniformly distributed throughout all three layers. Scanning electron microscopy and white light interferometry surface roughness measurements demonstrate that the formation of the layer occurs rapidly and, therefore provides an effective inhibition mechanism. Based on the observation of this work, a mechanism is proposed for the formation of these protective layers.

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