Specimen preparation for atom probe tomography analysis of complex multifunctional nanoparticles and nanostructures: state-of-the-art and challenges

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Main Authors: Nallathambi, Varatharaja, Kim, Se-Ho, Polin, Nikita, Shkodich, Natalia F., Reichenberger, Sven, Barcikowski, Stephan, Gault, Baptiste
Format: Preprint
Published: 2025
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author Nallathambi, Varatharaja
Kim, Se-Ho
Polin, Nikita
Shkodich, Natalia F.
Reichenberger, Sven
Barcikowski, Stephan
Gault, Baptiste
author_facet Nallathambi, Varatharaja
Kim, Se-Ho
Polin, Nikita
Shkodich, Natalia F.
Reichenberger, Sven
Barcikowski, Stephan
Gault, Baptiste
contents Atom probe tomography (APT) provides the three-dimensional composition of materials at near-atomic length scales, achieving detection limits in the range of tens of atomic parts-per-million regardless of element type. APT requires the specimen to be shaped as a needle with a tip radius of ~100 nm. The development of site-specific lift-out procedures using focused ion beam-scanning electron microscopy (FIB-SEM) has enabled APT analysis of multifunctional materials, advancing our understanding of their structure-composition-property relationships. Yet these approaches are not readily suitable for analyzing many nanomaterials. Co-electrodeposition of metallic films forms a composite containing the nanomaterials of interest, thereby facilitating APT specimen preparation and enabling analysis of nanowires, nanosheets, and nano- and microparticles, etc. In this perspective article, we showcase diverse examples from simple elementary to compositionally complex alloys of varying dimensionalities, from individual nanoparticles to aerogel structures. We emphasize the challenges encountered with specific material classes during co-electrodeposition procedures and provide recommendations for improving specimen preparation protocols to enhance measurement yield, thereby advancing APT analysis capabilities for optimizing the performance of functional nanomaterials.
format Preprint
id arxiv_https___arxiv_org_abs_2510_15629
institution arXiv
publishDate 2025
record_format arxiv
spellingShingle Specimen preparation for atom probe tomography analysis of complex multifunctional nanoparticles and nanostructures: state-of-the-art and challenges
Nallathambi, Varatharaja
Kim, Se-Ho
Polin, Nikita
Shkodich, Natalia F.
Reichenberger, Sven
Barcikowski, Stephan
Gault, Baptiste
Materials Science
Atom probe tomography (APT) provides the three-dimensional composition of materials at near-atomic length scales, achieving detection limits in the range of tens of atomic parts-per-million regardless of element type. APT requires the specimen to be shaped as a needle with a tip radius of ~100 nm. The development of site-specific lift-out procedures using focused ion beam-scanning electron microscopy (FIB-SEM) has enabled APT analysis of multifunctional materials, advancing our understanding of their structure-composition-property relationships. Yet these approaches are not readily suitable for analyzing many nanomaterials. Co-electrodeposition of metallic films forms a composite containing the nanomaterials of interest, thereby facilitating APT specimen preparation and enabling analysis of nanowires, nanosheets, and nano- and microparticles, etc. In this perspective article, we showcase diverse examples from simple elementary to compositionally complex alloys of varying dimensionalities, from individual nanoparticles to aerogel structures. We emphasize the challenges encountered with specific material classes during co-electrodeposition procedures and provide recommendations for improving specimen preparation protocols to enhance measurement yield, thereby advancing APT analysis capabilities for optimizing the performance of functional nanomaterials.
title Specimen preparation for atom probe tomography analysis of complex multifunctional nanoparticles and nanostructures: state-of-the-art and challenges
topic Materials Science
url https://arxiv.org/abs/2510.15629