A novel instrument for investigating the dynamic microstructure evolution of high temperature service materials up to 1150 °c in scanning electron microscope

Abstract

High temperature materials usually serve under extreme conditions. In order to ensure the safety and reliability of industrial application, it is very significant to clarify the microstructural evolution and mechanical properties at high temperature. The in situ experiment combining mechanical tensile testing and heating in the scanning electron microscope (SEM) is a feasible method to study the relationship between the microstructure, mechanical properties, and temperature. However, it was challenging to acquire images of high quality when the temperature exceeded 800 °C due to the effect of thermal electrons and the instability of loading conditions at high temperature. In this study, a mini-tensile apparatus was devised and installed in an ordinary SEM, which can achieve a stable loading of 0-2200 N and obtain high quality images in the temperature range of 1150 °C. A highly efficient heat source with multi-layer thermal insulation was designed to prevent the other parts of the apparatus from being affected by high temperature. A symmetrical tensile structure was developed to ensure that the region of interest was always within the field of view of the microscope during testing. Thermal electrons were suppressed to ensure that the sample can be clearly distinguished at 1150 °C. In order to ensure the testing reliability, standard carbon steel was used to calibrate the instrument. Finally, a Ni-based single crystal superalloy, as an example, was tested using this in situ tensile testing system at 1150 °C to verify the main functions and reliability of the apparatus.