A Technique for Real-Time, In-Situ SEM Observation of Grain Growth at Elevated Temperatures

Abstract

We present a novel electron detector and technique permitting orientation contrast images to be generated using back-scattered electron signals. The detector is a modification of the converter plate. It is unaffected by Infra-Red and light photons and invulnerable to the effects of heat. Consequently, the detector is removed as the temperature limiting factor in elevated temperature SEM grain observations. The detector has been successfully applied to an environmental SEM (ESEM) operating in high vacuum mode and has produced good quality video image sequences of hot metal specimens with frame rates between 1 per second and 1 per 30 seconds (largely material dependent). Temperatures attained were up to 850°C, limited by the capability of the hot stage. Although developed for the ESEM the technique is applicable to any SEM provided that adequate measures are taken to manage contamination and heat effects on other microscope components. We have produced images and short, accelerated video sequences of recrystallisation and grain growth phenomena in steel, aluminium, copper and gold by the new technique. The technique has also successfully imaged phase transformations and high temperature behaviour of microelectronic materials.