Advanced TEM specimen preparation methods for replication of P91 steel

Abstract

A range of advanced transmission electron microscopy specimen preparation methods, based on replication, have been developed for P91 steel. The results obtained have been compared with conventional replication and thin foil methods. The aim has been to obtain complimentary information from thin foil and replica specimens from the same region of interest either sequentially or simultaneously. The effects of various reagents for dissolution of the steel matrix and replica release have been investigated, and chemical methods for removing amorphous iron oxide contaminants from replicas have been identified. A method of region-specific replication is demonstrated whereby regions of thin foils previously characterised by TEM, can be subsequently replicated. This enables the former location of extracted particles, such as on grain/lath/subgrain boundaries etc., to be determined prior to microanalysis. It also permits the identification of artefacts such as stray particles and failed extractions. A second method of thin foil partial replication was developed in which both replica and thin foil are present on the same specimen. At the interface between the two regions, thin foil information such as dislocation interactions with fine scale particles and replica information such as microanalysis of particles within the same grain or lath can be obtained. Double replication of thin foils has also been successfully demonstrated. These methods are applied to a creep resistant martensitic steel (P91), but should be broadly applicable to a wide range of alloy steels.