Reliable Atom Probe Tomography of Cu Nanoparticles Through Tailored Encapsulation by an Electrodeposited Film
Nanoparticles are essential for energy storage, catalysis, and medical applications, emphasizing their accurate chemical characterization. However, atom probe tomography (APT) of nanoparticles sandwiched at the interface between an encapsulating film and a substrate poses difficulties. Poor adhesion...
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MDPI AG
2024-12-01
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| Series: | Nanomaterials |
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| Online Access: | https://www.mdpi.com/2079-4991/15/1/43 |
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| author | Aydan Çiçek Florian Knabl Maximilian Schiester Helene Waldl Lidija D. Rafailović Michael Tkadletz Christian Mitterer |
| author_facet | Aydan Çiçek Florian Knabl Maximilian Schiester Helene Waldl Lidija D. Rafailović Michael Tkadletz Christian Mitterer |
| author_sort | Aydan Çiçek |
| collection | DOAJ |
| description | Nanoparticles are essential for energy storage, catalysis, and medical applications, emphasizing their accurate chemical characterization. However, atom probe tomography (APT) of nanoparticles sandwiched at the interface between an encapsulating film and a substrate poses difficulties. Poor adhesion at the film-substrate interface can cause specimen fracture during APT, while impurities may introduce additional peaks in the mass spectra. We demonstrate preparing APT specimens with strong adhesion between nanoparticles and film/substrate matrices for successful analysis. Copper nanoparticles were encapsulated at the interface between nickel film and cobalt substrate using electrodeposition. Cobalt and nickel were chosen to match their evaporation fields with copper, minimizing peak overlaps and aiding nanoparticle localization. Copper nanoparticles were deposited via magnetron sputter inert gas condensation with varying deposition times to yield suitable surface coverages, followed by encapsulation with the nickel film. In-plane and cross-plane APT specimens were prepared by femtosecond laser ablation and focused ion beam milling. Longer deposition times resulted in agglomerated nanoparticles as well as pores and voids, causing poor adhesion and specimen failure. In contrast, shorter deposition times provided sufficient surface coverage, ensuring strong adhesion and reducing void formation. This study emphasizes controlled surface coverage for reliable APT analysis, offering insights into nanoparticle chemistry. |
| format | Article |
| id | doaj-art-e490dcad251d4a788af5ab59dbfa2a75 |
| institution | Kabale University |
| issn | 2079-4991 |
| language | English |
| publishDate | 2024-12-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Nanomaterials |
| spelling | doaj-art-e490dcad251d4a788af5ab59dbfa2a752025-01-10T13:19:20ZengMDPI AGNanomaterials2079-49912024-12-011514310.3390/nano15010043Reliable Atom Probe Tomography of Cu Nanoparticles Through Tailored Encapsulation by an Electrodeposited FilmAydan Çiçek0Florian Knabl1Maximilian Schiester2Helene Waldl3Lidija D. Rafailović4Michael Tkadletz5Christian Mitterer6Department of Materials Science, Montanuniversität Leoben, 8700 Leoben, AustriaDepartment of Materials Science, Montanuniversität Leoben, 8700 Leoben, AustriaDepartment of Materials Science, Montanuniversität Leoben, 8700 Leoben, AustriaDepartment of Materials Science, Montanuniversität Leoben, 8700 Leoben, AustriaDepartment of Materials Science, Montanuniversität Leoben, 8700 Leoben, AustriaDepartment of Materials Science, Montanuniversität Leoben, 8700 Leoben, AustriaDepartment of Materials Science, Montanuniversität Leoben, 8700 Leoben, AustriaNanoparticles are essential for energy storage, catalysis, and medical applications, emphasizing their accurate chemical characterization. However, atom probe tomography (APT) of nanoparticles sandwiched at the interface between an encapsulating film and a substrate poses difficulties. Poor adhesion at the film-substrate interface can cause specimen fracture during APT, while impurities may introduce additional peaks in the mass spectra. We demonstrate preparing APT specimens with strong adhesion between nanoparticles and film/substrate matrices for successful analysis. Copper nanoparticles were encapsulated at the interface between nickel film and cobalt substrate using electrodeposition. Cobalt and nickel were chosen to match their evaporation fields with copper, minimizing peak overlaps and aiding nanoparticle localization. Copper nanoparticles were deposited via magnetron sputter inert gas condensation with varying deposition times to yield suitable surface coverages, followed by encapsulation with the nickel film. In-plane and cross-plane APT specimens were prepared by femtosecond laser ablation and focused ion beam milling. Longer deposition times resulted in agglomerated nanoparticles as well as pores and voids, causing poor adhesion and specimen failure. In contrast, shorter deposition times provided sufficient surface coverage, ensuring strong adhesion and reducing void formation. This study emphasizes controlled surface coverage for reliable APT analysis, offering insights into nanoparticle chemistry.https://www.mdpi.com/2079-4991/15/1/43atom probe tomographynanoparticleselectrodepositionparticle encapsulation |
| spellingShingle | Aydan Çiçek Florian Knabl Maximilian Schiester Helene Waldl Lidija D. Rafailović Michael Tkadletz Christian Mitterer Reliable Atom Probe Tomography of Cu Nanoparticles Through Tailored Encapsulation by an Electrodeposited Film Nanomaterials atom probe tomography nanoparticles electrodeposition particle encapsulation |
| title | Reliable Atom Probe Tomography of Cu Nanoparticles Through Tailored Encapsulation by an Electrodeposited Film |
| title_full | Reliable Atom Probe Tomography of Cu Nanoparticles Through Tailored Encapsulation by an Electrodeposited Film |
| title_fullStr | Reliable Atom Probe Tomography of Cu Nanoparticles Through Tailored Encapsulation by an Electrodeposited Film |
| title_full_unstemmed | Reliable Atom Probe Tomography of Cu Nanoparticles Through Tailored Encapsulation by an Electrodeposited Film |
| title_short | Reliable Atom Probe Tomography of Cu Nanoparticles Through Tailored Encapsulation by an Electrodeposited Film |
| title_sort | reliable atom probe tomography of cu nanoparticles through tailored encapsulation by an electrodeposited film |
| topic | atom probe tomography nanoparticles electrodeposition particle encapsulation |
| url | https://www.mdpi.com/2079-4991/15/1/43 |
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