A nanocalorimeter designed for use with high-resolution transmission electron microscopy

Area of Science:

• Materials Science
• Analytical Chemistry
• Physical Chemistry

Background:

• Nanocalorimetry is a powerful thermal analysis technique for studying phase transformations and chemical reactions.
• Existing methods often lack the capability for simultaneous high-resolution imaging during rapid thermal measurements.

Purpose of the Study:

• To design and fabricate a nanocalorimeter compatible with transmission electron microscopes (TEMs) for in situ observations.
• To enable high-rate thermal measurements synchronized with high-speed imaging.

Main Methods:

• Development of a TEM-holder-compatible nanocalorimeter with electrical connections for in situ observation.
• Utilization of thin alumina and silicon nitride membranes as TEM observation windows.
• Fabrication of nanocalorimeters with perforations for direct specimen imaging in vacuum.

Main Results:

• Successful integration of nanocalorimetry with TEM for in situ observation during high-rate thermal analysis.
• Demonstrated high-resolution and high-speed imaging capabilities using 10 nm alumina and 20 nm silicon nitride membranes.
• Reduced background signal achieved by eliminating underlying support layers for specific specimens like thin gold films.

Conclusions:

• The developed nanocalorimeter offers a versatile platform for in situ TEM studies of thermal events.
• Coupling nanocalorimetry with high-frame-rate direct electron detectors allows for simultaneous thermal analysis and microstructure evolution monitoring.