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On-Tip Polymerization Method for Multimodal Characterization of Nanoparticles with Electron/Ion Imaging and Atom
Aristide Djoulde1, Anup Sharma1,2, Alfred Bekoe Appiagyei3
1Department of Mechanical and Aerospace Engineering, Monash University, Clayton, Victoria, 3800, Australia.
Small Methods
|May 26, 2025
Summary
A novel "needle-eye" technique precisely positions nanoparticles for advanced microscopy. This method enables detailed structural and chemical analysis of individual and clustered nanoparticles with unprecedented resolution.
Area of Science:
- Materials Science
- Nanotechnology
- Analytical Chemistry
Background:
- Correlative microscopy requires precise sample manipulation for multimodal analysis.
- Analyzing nanoparticle structures and chemistry presents significant challenges.
- Existing methods for nanoparticle preparation are often complex and time-consuming.
Purpose of the Study:
- To introduce a novel "needle-eye" method for nanoparticle exploration.
- To overcome limitations in multimodal and correlative microscopy of nanoparticles.
- To enable high-resolution structural and chemical imaging of nanoparticles.
Main Methods:
- Fabrication of a "needle-eye" microchannel at the needle tip using focused ion beam (FIB) milling and plasma treatment.
- Confinement of nanoparticles within the microchannel via a pressure gradient.
- In situ polymerization and shaping of nanoparticle samples into various geometries (micropillar, lamella, nanoneedle) using FIB.
- Characterization using energy-dispersive X-ray spectroscopy (EDX), FIB secondary ion mass spectrometry (FIB-SIMS), (scanning) transmission electron microscopy ((S)TEM), and atom probe tomography (APT).
Main Results:
- Demonstration of the "needle-eye" method's applicability using a mixed metal oxide catalyst.
- Successful multimodal analysis combining correlative and complementary high-resolution structural and chemical imaging.
- Validation of the method's ability to analyze individual and clustered nanoparticles.
- Efficient confinement of picoliter-scale samples (6-60 pL) at the needle tip.
Conclusions:
- The "needle-eye" method offers a streamlined approach for nanoparticle analysis.
- This technique eliminates the need for lift-out and microtomy, simplifying sample preparation.
- Enables comprehensive analysis of nanoparticles through combined microscopy techniques with high spatial resolution.
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