A quantitative determination of the polymerization of benzoxazine thin coatings by time‐of‐flight secondary ion mass spectrometry

Phenol‐paraphenylenediamine (P‐pPDA) benzoxazines exhibit excellent barrier properties, adequate to protect aluminum alloys from corrosion, and constitute interesting candidates to replace chromate‐containing coatings in the aeronautical industry. For the successful application of P‐pPDA coatings, i...

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Bibliographic Details
Published in:Surface and interface analysis 2019-06, Vol.51 (6), p.674-680
Main Authors: Pospisilova, Eva, Renaud, Alexis, Poorteman, Marc, Olivier, Marjorie, Dumas, Ludovic, Dubois, Philippe, Bonnaud, Leila, Moshkunov, Konstantin, Nysten, Bernard, Delcorte, Arnaud
Format: Article
Language:English
Subjects:
Aeronautics
Aluminum base alloys
Argon
benzoxazine
Benzoxazines
Bulk polymerization
Bulk sampling
Chromate coatings
crosslinking
Curing
Depth profiling
Differential scanning calorimetry
Ions
Mass spectrometry
Mechanical properties
Polymerization
Protective coatings
Scientific imaging
Secondary ion mass spectrometry
Spectroscopy
Thin films
thin polymer coatings
ToF‐SIMS
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Summary:Phenol‐paraphenylenediamine (P‐pPDA) benzoxazines exhibit excellent barrier properties, adequate to protect aluminum alloys from corrosion, and constitute interesting candidates to replace chromate‐containing coatings in the aeronautical industry. For the successful application of P‐pPDA coatings, it is necessary to decrease the curing temperature to avoid the delamination of the coating while preserving the mechanical properties of the alloy, as well as the barrier properties of the coating. However, decreasing the curing temperature leads to less polymerized films, the extent of which requires a quantitative assessment. While the conversion rate of the polymerization reaction is commonly evaluated for bulk samples using differential scanning calorimetry (DSC), a tool for its evaluation in thin films is missing. Therefore, a new approach was developed for that matter using time‐of‐flight secondary ion mass spectrometry (ToF‐SIMS). The relation between the SIMS data integrated from inside thin films and the DSC results obtained on bulk samples with the same curing cycle allowed to calibrate the SIMS data. With this preliminary calibration of the technique, the polymerization of P‐pPDA coatings can be locally determined, at the surface and along the depth of the coating, using dual‐beam depth profiling with large argon cluster beam sputtering.
ISSN:0142-2421
1096-9918
DOI:10.1002/sia.6639