Nanoscale analysis of frozen honey by atom probe tomography

Schwarz, Tim; Ott, Jonas; Solodenko, Helena; Schmitz, Guido; Stender, Patrick

doi:10.1038/s41598-022-22717-9

Cited by 4 publications

(1 citation statement)

References 66 publications

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“…In recent years, the development of cryogenic transfer systems for sample transfer between different instruments has made it possible to transfer samples from the glove box to the cryo-focused ion beam (FIB) and then to the atom probe for analysis. [35,36] Cryo-APT has made it possible to study frozen liquids by APT, [37][38][39][40][41] along with liquid-solid interfaces, enabling, e.g., the study of glass corrosion reaction fronts. [42] Here we introduce cryo-APT as a quasi-"in situ" approach to study the reaction front of Mg alloy used as a biodegradable implant during aqueous corrosion to analyze the early-stage corrosion mechanism and the diffusion of alloying elements.…”

Section: Introductionmentioning

confidence: 99%

Quasi‐“In Situ” Analysis of the Reactive Liquid‐Solid Interface during Magnesium Corrosion Using Cryo‐Atom Probe Tomography

Schwarz,

Yang,

Aota

et al. 2024

Advanced Materials

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The early stages of corrosion occurring at liquid‐solid interfaces controls the evolution of the material's degradation process, yet due to their transient state, their analysis remains a formidable challenge. Here we perform corrosion tests on a MgCa alloy, a candidate material for biodegradable implants using pure water as a model system. The corrosion reaction was suspended by plunge freezing into liquid nitrogen. We studied the evolution of the early‐stage corrosion process on the nanoscale by correlating cryo‐atom probe tomography with transmission‐electron microscopy and spectroscopy. We observed the outward growth of Mg hydroxide and the inward growth of an intermediate corrosion layer consisting of hydroxides of different compositions, mostly monohydroxide Mg(OH) instead of the expected MgO layer. In addition, Ca partitions to these newly formed hydroxides and oxides. Density‐functional theory calculations suggest a domain of stability for this previously experimental unreported Mg(OH) phase. These new approach and findings advance the understanding of the early stages of magnesium corrosion, and in general reactions and processes at liquid‐solid interfaces, which can further facilitate the development of corrosion‐resistant materials or better control of the biodegradation rate of future implants.This article is protected by copyright. All rights reserved

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Section: Introductionmentioning

confidence: 99%

Quasi‐“In Situ” Analysis of the Reactive Liquid‐Solid Interface during Magnesium Corrosion Using Cryo‐Atom Probe Tomography

Schwarz,

Yang,

Aota

et al. 2024

Advanced Materials

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Nanoscale Analysis of Frozen Water by Atom Probe Tomography Using Graphene Encapsulation and Cryo-Workflows

Exertier,

Tegg,

Taylor

et al. 2024

Microscopy and Microanalysis

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There has been an increasing interest in atom probe tomography (APT) to characterize hydrated and biological materials. A major benefit of APT compared to microscopy techniques more commonly used in biology is its combination of outstanding three-dimensional (3D) spatial resolution and mass sensitivity. APT has already been successfully used to characterize biominerals, revealing key structural information at the atomic scale, however there are many challenges inherent to the analysis of soft hydrated materials. New preparation protocols, often involving specimen preparation and transfer at cryogenic temperature, enable APT analysis of hydrated materials and have the potential to enable 3D atomic scale characterization of biological materials in the near-native hydrated state. In this study, samples of pure water at the tips of tungsten needle specimens were prepared at room temperature by graphene encapsulation. A comparative study was conducted where specimens were transferred at either room temperature or cryo-temperature and analyzed by APT by varying the flight path and pulsing mode. The differences between the analysis workflows are presented along with recommendations for future studies, and the compatibility between graphene coating and cryogenic workflows is demonstrated.

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Analysis of Water Ice in Nanoporous Copper Needles Using Cryo Atom Probe Tomography

Tegg,

McCarroll,

Kim

et al. 2024

Microscopy and Microanalysis

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The application of atom probe tomography (APT) to frozen liquids is limited by difficulties in specimen preparation. Here, we report on the use of nanoporous Cu needles as a physical framework to hold water ice for investigation using APT. Nanoporous Cu needles are prepared by electropolishing and dealloying Cu–Mn matchstick precursors. Cryogenic scanning electron microscopy and focused ion beam milling reveal a hierarchical, dendritic, highly wettable microstructure. The atom probe mass spectrum is dominated by peaks of Cu+ and H(H2O)n+ up to n ≤ 3, and the reconstructed volume shows the protrusion of a Cu ligament into an ice-filled pore. The continuous Cu ligament network electrically connects the apex to the cryostage, leading to an enhanced electric field at the apex and increased cooling, both of which simplify the mass spectrum compared to previous reports.

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Nanoscale analysis of frozen honey by atom probe tomography

Cited by 4 publications

References 66 publications

Quasi‐“In Situ” Analysis of the Reactive Liquid‐Solid Interface during Magnesium Corrosion Using Cryo‐Atom Probe Tomography

Quasi‐“In Situ” Analysis of the Reactive Liquid‐Solid Interface during Magnesium Corrosion Using Cryo‐Atom Probe Tomography

Nanoscale Analysis of Frozen Water by Atom Probe Tomography Using Graphene Encapsulation and Cryo-Workflows

Analysis of Water Ice in Nanoporous Copper Needles Using Cryo Atom Probe Tomography

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