MEMS-based Heating Element for in-situ Dynamical Experiments on FIB/SEM Systems

In-situ observation of microstructural evolution of solids such as recrystallization, grain growth and phase changes in SEM is important for various fields of material science and industry research. This technique requires reliable discrimination of differently oriented crystal phases combined with useful spatial and temporal resolution and with fast and precise control of specimen temperature. While the requirements on spatial and temporal resolution are satisfied by current SEMs with resolution below 1 nm and 100 Hz frame rate, existing heating holders for bulk samples only allow for heating rates up to 300C per minute (5C/s). Long ramping time, which is required during heating experiments done using these devices, may cause unwanted sample changes (e.g. oxidation or recrystallization) before the temperature range of interest is reached. Thermal radiation of massive heating holders decreases quality of material contrast imaging as the commonly used detectors of backscattered electrons become saturated by thermally emitted photons. MEMS-based heating holder 1, 2 in combination with in-situ site specific sample preparation using a FIB/SEM system brings significant improvement in instrumentation for in-situ heating experiments inside the SEM chamber.