Facilitating Atom Probe Tomography of 2D MXene Films by In Situ Sputtering

Area of Science:

• Materials Science
• Nanotechnology
• Chemistry

Background:

• Two-dimensional (2D) materials, including MXenes, are vital nanomaterials for energy storage and catalysis.
• Wet chemical synthesis of MXenes results in diverse functional groups and requires intercalating cations like Li+ for exfoliation.
• Understanding the precise chemical composition of synthesized 2D materials is essential for correlating structure with properties.

Purpose of the Study:

• To present a revised specimen preparation method for atom probe tomography (APT) analysis of 2D materials.
• To enable detailed chemical composition analysis of MXenes and similar 2D materials.
• To facilitate the study of structure-property relationships in advanced nanomaterials.

Main Methods:

• A colloidal Ti3C2Tz MXene solution was processed into an additive-free, free-standing film.
• Specimen preparation for APT was performed using a dual-beam scanning electron microscope/focused ion beam (FIB-SEM).
• An in situ sputtering technique was employed to mechanically stabilize fragile specimens.

Main Results:

• The study successfully prepared MXene specimens suitable for APT analysis.
• The revised method allows for detailed chemical composition determination of 2D materials.
• The technique demonstrated the potential for analyzing other 2D material inks processed into films.

Conclusions:

• The presented specimen preparation method is crucial for advancing APT analysis of 2D materials.
• This approach will enhance the understanding of composition-property relationships in MXenes and other 2D nanomaterials.
• The technique opens new avenues for materials characterization in energy storage and catalysis research.