The Performance of EDXS at Elevated Sample Temperatures Using a MEMS-Based In Situ TEM Heating System.

Area of Science:

• Materials Science
• Analytical Chemistry
• Physics

Background:

• Microelectromechanical Systems (MEMS) heating holders enable dynamic in situ experiments at elevated temperatures.
• These holders can be coupled with X-ray spectrometry for chemical analysis.
• Infrared (IR) radiation from heating devices can affect X-ray spectral quality.

Purpose of the Study:

• To systematically investigate the influence of IR radiation from MEMS heating systems on energy-dispersive X-ray (EDX) spectra.
• To analyze the impact of holder geometry, shadowing, and orientation on IR and X-ray photon interactions.
• To provide a guide for optimizing in situ heating experiments for chemical EDXS analysis.

Main Methods:

• Simulations and experimental measurements were employed to examine IR radiation effects.
• The study focused on DENSsolutions single- and double-tilt holders.
• Interactions with side-entry and multi-detector systems were considered.

Main Results:

• IR photons significantly increase count rates, dead time, and electronic noise.
• IR radiation negatively affects energy resolution and detector efficiency.
• At higher temperatures, IR radiation limits elemental characterization, especially for low-Z elements.

Conclusions:

• IR radiation from MEMS heating holders is a critical factor influencing EDXS data quality.
• Understanding these influences is crucial for accurate elemental analysis during in situ heating.
• Optimization strategies are needed to mitigate IR effects for reliable in situ chemical characterization.