A new method for mapping the three-dimensional atomic distribution within nanoparticles by atom probe tomography (APT)

Kim, Se‐Ho; Kang, Phil Woong; Park, O Ok; Seol, Jae Bok; Ahn, Jae‐Pyoung; Lee, Jiyeong; Choi, Pyuck‐Pa

doi:10.1016/j.ultramic.2018.04.005

Cited by 58 publications

(54 citation statements)

References 57 publications

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“…Preparation of the goethite microrods into needle-shaped tips is challenging but necessary for APT analysis. Currently, there are few successful approaches for the preparation of APT specimens from unsupported nanostructured materials that result in meaningful APT results (28)(29)(30)(31)(32). The goethite microrods in our study were prepared for APT analysis using an encapsulation, cross-sectioning approach (33).…”

Section: Resultsmentioning

confidence: 99%

“…Although challenging, APT analysis of the distribution of potassium on amorphous ferrihydrite particles was previously achieved (31). In particular, nanoparticles must be embedded in a matrix without nanovoids or microvoids, which can cause premature fracture or artifacts in APT reconstructions, that preserves their structure and composition to acquire meaningful data that can be related to the original particles (32,51,52). Tedious but essential work entails refining and testing specimen preparation techniques, such as embedding in a material compatible with field ionization of the particles that is free of voids, strongly adhered, and free of noninterfering ions.…”

Section: Discussionmentioning

confidence: 99%

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Visualizing the iron atom exchange front in the Fe(II)-catalyzed recrystallization of goethite by atom probe tomography

Taylor

Liu

Zhang

et al. 2019

Proc. Natl. Acad. Sci. U.S.A.

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The autocatalytic redox interaction between aqueous Fe(II) and Fe(III)-(oxyhydr)oxide minerals such as goethite and hematite leads to rapid recrystallization marked, in principle, by an atom exchange (AE) front, according to bulk iron isotopic tracer studies. However, direct evidence for this AE front has been elusive given the analytical challenges of mass-resolved imaging at the nanoscale on individual crystallites. We report successful isolation and characterization of the AE front in goethite microrods by 3D atom probe tomography (APT). The microrods were reacted with Fe(II) enriched in tracer 57Fe at conditions consistent with prior bulk studies. APT analyses and 3D reconstructions on cross-sections of the microrods reveal an AE front that is spatially heterogeneous, at times penetrating several nanometers into the lattice, in a manner consistent with defect-accelerated exchange. Evidence for exchange along microstructural domain boundaries was also found, suggesting another important link between exchange extent and initial defect content. The findings provide an unprecedented view into the spatial and temporal characteristics of Fe(II)-catalyzed recrystallization at the atomic scale, and substantiate speculation regarding the role of defects controlling the dynamics of electron transfer and AE interaction at this important redox interface.

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Section: Resultsmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%

Visualizing the iron atom exchange front in the Fe(II)-catalyzed recrystallization of goethite by atom probe tomography

Taylor

Liu

Zhang

et al. 2019

Proc. Natl. Acad. Sci. U.S.A.

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“…As‐synthesized MoS 2 nanosheets were electrodeposited within Ni film for embedding nanoparticles according to Kim et al Nickel sulfate hexahyrdrate (NiSO 4 ⋅6H 2 O, Sigma‐Aldrich (Germany)), and boric acid (H 3 BO 3 , Sigma‐Aldrich (Germany)) were dissolved in distilled water. The nanosheets were then dispersed in as‐prepared electrolyte solution and poured in a vertical cell for co‐electrodeposition process.…”

Section: Methodsmentioning

confidence: 99%

“…We used co‐electrodeposition of a Ni‐film to embed freestanding Re‐MoS 2 nanosheets, applying the method described in ref. , so as to enable the preparation of a sharp specimens (<100 nm at the apex). A similar approach had previously been used for nanoparticles, but never for 2D materials.…”

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confidence: 99%

Direct Imaging of Dopant and Impurity Distributions in 2D MoS₂

et al. 2020

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Molybdenum disulfide (MoS2) nanosheet is a two‐dimensional (2D) material with high electron mobility and with high potential for applications in catalysis and electronics. MoS2 nanosheets are synthesized using a one‐pot wet‐chemical synthesis route with and without Re doping. Atom probe tomography reveals that 3.8 at% Re is homogeneously distributed within the Re‐doped sheets. Other impurities are also found integrated within the material: light elements including C, N, O, and Na, locally enriched up to 0.1 at%, as well as heavy elements such as V and W. Analysis of the nondoped sample reveals that the W and V likely originate from the Mo precursor. It is shown how wet‐chemical synthesis results in an uncontrolled integration of species from the solution that can affect the material's activity. The results of this work are expected to contribute to an improved understanding of the relationships linking composition to properties of 2D transition‐metal dichalcogenide materials.

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“…Finally, Pd and Csupported Pt nanoparticles were analyzed by APT using a methodology consisting of the electrophoretic deposition of nanoparticles on a flat Cu substrate followed by electrodeposition of a Ni film acting as an embedding matrix for the nanoparticles. Reliable APT data could be obtained for Pd nanoparticles, but the carbon-based support leads to artifacts [134]. All these alternate methods Alternative encapsulation methods have been used to analyze nanomaterials but could be extended to catalytic materials.…”

Section: Alternative Encapsulation Methods Have Been Used To Analyze mentioning

confidence: 99%

Atom Probe Tomography for Catalysis Applications: A Review

2019

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Atom probe tomography is a well-established analytical instrument for imaging the 3D structure and composition of materials with high mass resolution, sub-nanometer spatial resolution and ppm elemental sensitivity. Thanks to recent hardware developments in Atom Probe Tomography (APT), combined with progress on site-specific focused ion beam (FIB)-based sample preparation methods and improved data treatment software, complex materials can now be routinely investigated. From model samples to complex, usable porous structures, there is currently a growing interest in the analysis of catalytic materials. APT is able to probe the end state of atomic-scale processes, providing information needed to improve the synthesis of catalysts and to unravel structure/composition/reactivity relationships. This review focuses on the study of catalytic materials with increasing complexity (tip-sample, unsupported and supported nanoparticles, powders, self-supported catalysts and zeolites), as well as sample preparation methods developed to obtain suitable specimens for APT experiments.

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A new method for mapping the three-dimensional atomic distribution within nanoparticles by atom probe tomography (APT)

Cited by 58 publications

References 57 publications

Visualizing the iron atom exchange front in the Fe(II)-catalyzed recrystallization of goethite by atom probe tomography

Visualizing the iron atom exchange front in the Fe(II)-catalyzed recrystallization of goethite by atom probe tomography

Direct Imaging of Dopant and Impurity Distributions in 2D MoS₂

Atom Probe Tomography for Catalysis Applications: A Review

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A new method for mapping the three-dimensional atomic distribution within nanoparticles by atom probe tomography (APT)

Cited by 58 publications

References 57 publications

Visualizing the iron atom exchange front in the Fe(II)-catalyzed recrystallization of goethite by atom probe tomography

Visualizing the iron atom exchange front in the Fe(II)-catalyzed recrystallization of goethite by atom probe tomography

Direct Imaging of Dopant and Impurity Distributions in 2D MoS2

Atom Probe Tomography for Catalysis Applications: A Review

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Product

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Direct Imaging of Dopant and Impurity Distributions in 2D MoS₂