Temperature control - Material SEM

Method Specification

Temperature control of samples in SEM is used for different applications, among them water condensation and evaporation, particles thermal migration, phase transformation, in situ synthesis, low temperature spectroscopy and more. The sample’s temperature in the SEM can be controlled by special stages for heating or cooling.
High temperature experiments in situ SEM can be of great importance for materials characterization. Thermal stability of inorganic compounds, surface crystallization mechanisms and other dynamic processes can be detected in real time.  By heating a sample in situ SEM, one can directly observe the microstructure evolution during heating and/or cooling and record dynamical processes occurring on the surface. Special heating modules have been developed to heat samples up to 1400°C directly in the microscope chamber. Many studies have shown that an ESEM equipped with a heating stage is an excellent tool for the in situ and continuous observation of system modifications involved temperature. It allows recording image series of the morphological changes of a sample during a heat treatment with both high magnification and high depth of focus. The experiments can be carried out to observe the influence of all these parameters on the studied phenomenon under various conditions (heating rates, atmosphere compositions, variable pressure, final temperature and heating time).
Temperature control is also required to cool down samples when working in wet mode. In that case the condensation/evaporation of water can be controlled by a Peltier cooling stage (-20°C-60°C). High temperature experiments are mostly performed on inorganic materials as moderate low temperature experiments can be performed on organic and inorganic materials.
Cryo SEM in materials science is used to cool down solid samples inside the microscope. The samples can be cooled down by a cryo stage using LN. The temperature can be decreased down to -150°C. Solid samples can be cooled down for spectroscopical measurements such as EDS (energy dispersive x-ray spectroscopy) or CL (cathodoluminescence) under low temperatures. 

References

Instruments

  • RT - 1400°C heating module by Thermo Fisher Scientific installed on the Quattro S
  • RT - 1000°C high vacuum heating module by Thermo Fisher Scientific installed on the Quattro S
  • -20 - 60°C heating/cooling module by Thermo Fisher Scientific installed on the Quattro S
  • Cryo stage -150°C - RT by Leica installed on the Zeiss Gemini SEM 500 and on the Zeiss Ultra 55