Development of a microfurnace dedicated to in situ scanning electron microscope observation up to 1300 °C. II. Study of the thermal response of samples.

Abstract

When conducting in situ experiments at high temperatures in a scanning electron microscope using microfurnaces, controlling the temperature of a sample of a few mm3 placed in the hot zone of the furnace can be a complex task. In most cases, the temperature of the sample is estimated by means of a thermocouple placed in the hot body of the furnace, and the assumption made is that the temperature of the furnace is the temperature of the sample. In this work, a detailed understanding of the thermal response of the sample placed in the hot zone of the furnace is proposed. Temperature differences due to contact resistance between the furnace surface and the sample, the nature of the sample, and the sample geometry are calculated with a numerical model and measured experimentally on a dedicated test bench. Three technical solutions (bonding, sandwiching, and mini-crucible) for limiting temperature differences between the furnace surface and sample are proposed and validated by numerical calculations and experimental measurements.