Observations des mécanismes locaux d’endommagement

Après avoir analysé le comportement mécanique des composites SiC/SiC et C/SiC par essais de traction et push-out, les fibres indentées ou déchaussées au sein des composites sont extraites par FIB (figure II.21). Une étude par METHR est réalisée afin de déterminer l’évolution de la structure des interphases carbonées après essais mécaniques ainsi que la région à l’origine de la décohésion F/M. Ces observations pourront amener à une meilleure compréhension de la différence d’intensité du couplage F/M des composites SiC/SiC et C/SiC.

Figure II.21 - Lame mince obtenue par FIB d’une fibre SiC indentée au sein d’un composite SiC/PyC/SiC après essai push-out

6. CONCLUSION

Ce chapitre aborde les différentes techniques utilisées afin de caractériser l’extrême surface des fibres SiC et de carbone étudiées ainsi que les régions interfaciales des composites qu’elles renforcent.

Dans un premier temps, la composition de l’extrême surface des fibres est évaluée par analyses physico-chimiques. L’analyse thermogravimétrique couplée à la spectrométrie de masse (ATG- MS) des fibres apporte des informations sur le désensimage de la fibre, première étape réalisée lors de la densification des composites. Des renseignements sur la réactivité et la nature des sites actifs présents en surface de fibres sont fournis par chromatographie gazeuse inverse à dilution infinie (CGI-DI) et par spectroscopie de photoélectrons.

5 μm Matrice SiC Fibre SiC indentée PyC

CONFIDENTIEL CEA – REPRODUCTION INTERDITE 58 L’organisation microstructurale de la surface des fibres et des premières couches de pyrocarbone est examinée par microscopie électronique en transmission, principalement en haute résolution, aux différentes étapes de fabrication des composites SiC/SiC et C/SiC. Plusieurs méthodes (PIPS, FIB, Ion Slicer) sont utilisées pour préparer les lames minces de fibres et de composites. Les différents artéfacts générés par ces méthodes sont identifiés pour ne pas être associés à la microstructure de l’échantillon et entraîner de fausses interprétations. Après observation de ces échantillons, les clichés pris en haute résolution sont traités par des outils de caractérisation morphologique basés sur la morphologie mathématique. Des informations quantitatives sur l’arrangement spatial des plans de graphène sont obtenus, à la fois en surface de fibres mais aussi aux interphases des composites.

Par la suite, l’étude des propriétés mécaniques des composites SiC/SiCet C/SiC permet d’établir un lien entre la tolérance à la déformation des composites et la structure de la surface des fibres. Les caractéristiques mécaniques des composites sont comparées par des essais de traction monotone et cyclée en fonction de la nature des fibres et de la présence ou l’absence de l’interphase de pyrocarbone. Les propriétés interfaciales des composites sont quant à elles déterminées par essais push-out et de microdureté.

Ces caractérisations chimiques, microstructurales et mécaniques seront menées pour mieux comprendre l’influence des paramètres de surface de fibres qui conduisent au comportement mécanique des composites renforcés par les fibres TSA3. Suite à ces analyses, des solutions innovantes seront proposées pour optimiser le couplage fibre/matrice de ces composites.

CONFIDENTIEL CEA – REPRODUCTION INTERDITE 59

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