Development of a microfurnace dedicated to in situ scanning electron microscope observation up to 1300 °C. III. In situ high temperature experiments.

The FurnaSEM microfurnace was installed in the chamber of a scanning electron microscope to carry out in situ experiments at high temperatures and test its limits. The microfurnace was used in combination with different types of detectors (Everhart-Thornley for the collection of secondary electrons in a high vacuum, gas secondary electron detector for the specific collection of secondary electrons in the presence of gas, and Karmen© detector for the collection of backscattered electrons at high temperature). Experiments carried out on various samples (metal alloys and ceramics) show that the microfurnace operates in both high-vacuum and low-vacuum modes.

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

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.

Development of a microfurnace dedicated to in situ scanning electron microscope observation up to 1300 °C. I. Concept, fabrication, and validation.

The development of a new heating system dedicated to in situ scanning electron microscope (SEM) experimentation at high temperatures is reported. This system, called FurnaSEM, is a compact microfurnace, enabling heat treatments up to 1300 °C. The choice of materials for the microfurnace is explained.

Direct Observation of the Surface Topography at High Temperature with SEM.

High-temperature scanning electron microscopy allows the direct study of the temperature behavior of materials. Using a newly developed heating stage, tilted images series were recorded at high temperature and 3D images of the sample surface were reconstructed. By combining 3D images recorded at different temperatures, the variations of material roughness can be accurately described and associated with local changes in the topography of the sample surface.