Processing APT Spectral Backgrounds for Improved Quantification

Haley, Daniel; London, Andrew J.; Moody, Michael P.

doi:10.1017/s1431927620024290

Cited by 12 publications

(8 citation statements)

References 17 publications

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“…This indicates a negligible solubility of Nb in Mg 3 Sb 2 given the high elemental sensitivity of APT. [ 18 ] The high density of atoms at the interface is attributed to the local magnification effect during the APT measurement. [ 17a ] A composition profile was computed as a function of the distance to the iso‐composition surface delineating regions containing 30 at% Mg or more, and is plotted in Figure 3c.…”

Section: Nb Wetting and Interfacial Composition Characterized By Aptmentioning

confidence: 99%

Nb‐Mediated Grain Growth and Grain‐Boundary Engineering in Mg₃Sb₂‐Based Thermoelectric Materials

Luo

Kuo

Griffith

et al. 2021

Adv Funct Materials

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The poor carrier mobility of polycrystalline Mg3Sb2 at low temperatures strongly degrades the thermoelectric performance. Ionized impurities are initially thought to dominate charge carrier scattering at low temperatures. Accordingly, the increased electrical conductivity by replacing Mg with metals such as Nb is also attributed to reduced ionized impurity scattering. Recent experimental and theoretical studies challenge this view and favor the grain boundary (GB) scattering mechanism. A reduction of GB scattering improves the low‐temperature performance of Mg3(Sb, Bi)2 alloys. However, it is still elusive how these metal additions reduce the GB resistivity. In this study, Nb‐free and Nb‐added Mg3Sb2 are studied through diffraction, X‐ray absorption spectroscopy, solid‐state nuclear magnetic resonance spectroscopy, and atom probe tomography. It is shown that Nb does not enter the Mg3Sb2 matrix and remains in the metallic state. Besides, Nb diffuses along the GB forming a wetting layer, which modifies the interfacial energy and accelerates grain growth. The GB resistivity appears to be reduced by Nb‐enrichment, as evidenced by modeling the electrical transport properties. This study not only confirms the GB scattering in Mg3Sb2 but also reveals the hitherto hidden role of metallic additives on enhancing grain growth and reducing the GB resistivity.

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Section: Nb Wetting and Interfacial Composition Characterized By Aptmentioning

confidence: 99%

Nb‐Mediated Grain Growth and Grain‐Boundary Engineering in Mg₃Sb₂‐Based Thermoelectric Materials

Luo

Kuo

Griffith

et al. 2021

Adv Funct Materials

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“…It is critical to minimize the background level to maximize the sensitivity of the APT analysis of aqueous solutions. There is no unique definition of the detection sensitivity in APT, and multiple approaches already exist to provide numerical estimates (6,8). A metric for the compositional sensitivity should combine the mass resolution, i.e., how high a mass peak is for a given number of detected ions, the number of stable isotopes that lead to lower peak amplitude potentially, and also the local level of background that could obscure this specific set of peaks.…”

Section: Aspects Of the Apt Analysis Of Ice And Performance Limitsmentioning

confidence: 99%

“…Atom probe tomography (APT) is a burgeoning technique that enables three-dimensional (3D) elemental mapping (6) with subnanometer resolution (7) and a chemical sensitivity potentially down to only tens of parts per million (ppm) (8). The usefulness of APT in studying wet chemical systems has been limited by the challenges inherent to the analysis of liquid media.…”

Section: Introductionmentioning

confidence: 99%

Enabling near-atomic–scale analysis of frozen water

et al. 2020

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Transmission electron microscopy went through a revolution enabling routine cryo-imaging of biological and (bio)chemical systems, in liquid form. Yet, these approaches typically lack advanced analytical capabilities. Here, we used atom probe tomography to analyze frozen liquids in three dimensions with subnanometer resolution. We introduce a specimen preparation strategy using nanoporous gold. We report data on 2- to 3-μm-thick layers of ice formed from both high-purity deuterated water and a solution of 50 mM NaCl in high-purity deuterated water. The analysis of the gold-ice interface reveals a substantial increase in the solute concentrations across the interface. We explore a range of experimental parameters to show that atom probe analyses of bulk aqueous specimens come with their own challenges and discuss physical processes that produce the observed phenomena. Our study demonstrates the viability of using frozen water as a carrier for near-atomic–scale analysis of objects in solution by atom probe tomography.

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“…33,50,57 This can lead to components and phases with a low volume fraction to be missed or overlooked, yet their influence on the materials properties may remain substantial. This is where the correlation with APT can become a game changer: APT provides compositional mapping in three dimensions within the reconstructed volume, with a compositional sensitivity that can be in the range of parts-per-million, 58 individual features can be interrogated separately after data reconstruction and segmentation. This information can then be used to better understand the origins of the signal in the XPS or EELS spectrum.…”

Section: Complementarities and Challengesmentioning

confidence: 99%

Correlating atom probe tomography with x-ray and electron spectroscopies to understand microstructure–activity relationships in electrocatalysts

et al. 2022

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The search for a new energy paradigm with net-zero carbon emissions requires new technologies for energy generation and storage that are at the crossroad between engineering, chemistry, physics, surface, and materials sciences. To keep pushing the inherent boundaries of device performance and lifetime, we need to step away from a cook-and-look approach and aim to establish the scientific ground to guide the design of new materials. This requires strong efforts in establishing bridges between microscopy and spectroscopy techniques, across multiple scales. Here, we discuss how the complementarities of x-ray- and electron-based spectroscopies and atom probe tomography can be exploited in the study of surfaces and subsurfaces to understand structure–property relationships in electrocatalysts. Graphical abstract

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Processing APT Spectral Backgrounds for Improved Quantification

Abstract: Abstract

Cited by 12 publications

References 17 publications

Nb‐Mediated Grain Growth and Grain‐Boundary Engineering in Mg₃Sb₂‐Based Thermoelectric Materials

Nb‐Mediated Grain Growth and Grain‐Boundary Engineering in Mg₃Sb₂‐Based Thermoelectric Materials

Enabling near-atomic–scale analysis of frozen water

Correlating atom probe tomography with x-ray and electron spectroscopies to understand microstructure–activity relationships in electrocatalysts

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Processing APT Spectral Backgrounds for Improved Quantification

Abstract: Abstract

Cited by 12 publications

References 17 publications

Nb‐Mediated Grain Growth and Grain‐Boundary Engineering in Mg3Sb2‐Based Thermoelectric Materials

Nb‐Mediated Grain Growth and Grain‐Boundary Engineering in Mg3Sb2‐Based Thermoelectric Materials

Enabling near-atomic–scale analysis of frozen water

Correlating atom probe tomography with x-ray and electron spectroscopies to understand microstructure–activity relationships in electrocatalysts

Contact Info

Product

Resources

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Nb‐Mediated Grain Growth and Grain‐Boundary Engineering in Mg₃Sb₂‐Based Thermoelectric Materials

Nb‐Mediated Grain Growth and Grain‐Boundary Engineering in Mg₃Sb₂‐Based Thermoelectric Materials