Atomic-scale characterization of (electro-)catalysts and battery materials by atom probe tomography

Li, Tong; Devaraj, Arun; Kruse, Norbert

doi:10.1016/j.xcrp.2022.101188

Cited by 10 publications

(8 citation statements)

References 76 publications

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“…[13,14] Battery materials are also often reactive oxides, that require careful handling and sample transfer. [15] There are only few studies of battery materials using APT, as recently reviewed by Li et al [16] and more worryingly maybe, there are discrepancies between results, owing to these issues. [17][18][19][20] It is also important to acknowledge that compositional inhomogeneity at the micro or nano-scale, particularly in bulk prepared samples, can also cause such variations in the results.…”

Section: Introductionmentioning

confidence: 99%

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Facilitating the Systematic Nanoscale Study of Battery Materials by Atom Probe Tomography through in‐situ Metal Coating

Singh,

Woods,

Kim

et al. 2023

Batteries & Supercaps

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Through its capability for 3D mapping of Li at the nanoscale, atom probe tomography (APT) is poised to play a key role in understanding the microstructural degradation of lithium‐ion batteries (LIB) during successive charge‐ and discharge cycles. However, APT application to materials for LIB is plagued by the field induced delithiation (deintercalation) of Li‐ions during the analysis itself that prevents the precise assessment of the Li distribution. Here, we showcase how a thin Cr‐coating, in‐situ formed on APT specimens of NMC811 in the focused‐ion beam (FIB), preserves the sample’s integrity and circumvent this deleterious delithiation. Cr‐coated specimens demonstrated remarkable improvements in data quality and virtually eliminated premature specimen failures, allowing for more precise measurements via. improved statistics. Through improved data analysis, we reveal substantial cation fluctuations in commercial grade NMC811, including complete grains of LiMnO. The current methodology stands out for its simplicity and cost‐effectiveness and is a viable approach to prepare battery cathodes and anodes for systematic APT studies.

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Section: Introductionmentioning

confidence: 99%

“…Battery materials are also often reactive oxides, that require careful handling and sample transfer [15] . There are only few studies of battery materials using APT, as recently reviewed by Li et al [16] . and more worryingly maybe, there are discrepancies between results, owing to these issues [17–20] .…”

Section: Introductionmentioning

confidence: 99%

Facilitating the Systematic Nanoscale Study of Battery Materials by Atom Probe Tomography through in‐situ Metal Coating

Singh,

Woods,

Kim

et al. 2023

Batteries & Supercaps

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“…Since the measurement probes only a very small portion (few nanometers) of the cathode, the sample may not be representative of the entire surface. Despite these challenges, APT has the unique ability to map both heavy and light elements with high chemical sensitivity (0.01–0.1% elemental concentration) and subnanometer resolution (∼0.2–0.5 nm), making the technique one of the highest resolution characterization techniques accessible for CEI studies …”

Section: Profiling the Cei Structure From The Cathode Surface To The ...mentioning

confidence: 99%

“…Despite these challenges, APT has the unique ability to map both heavy and light elements with high chemical sensitivity (0.01−0.1% elemental concentration) and subnanometer resolution (∼0.2−0.5 nm), making the technique one of the highest resolution characterization techniques accessible for CEI studies. 101 2.4. Insights into the CEI Gained from Depth-Resolved Techniques.…”

Section: Atom-probe Tomography (Apt)mentioning

confidence: 99%

Beyond Composition: Surface Reactivity and Structural Arrangement of the Cathode–Electrolyte Interphase

Hestenes,

Marbella

2023

ACS Energy Lett.

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The role of the cathode–electrolyte interphase (CEI) on battery performance has been historically overlooked due to the anodic stability of carbonate-based electrolytes used in Li-ion batteries. Yet, over the past few decades, degradation in device lifetime has been attributed to cathode surface reactivity, ion transport at the cathode/electrolyte interface, and structural transformations that occur at the cathode surface. In this review, we highlight recent progress in analytical techniques that have facilitated these insights and elucidated not only the CEI composition but also the spatial distribution of electrolyte decomposition products in the CEI as well as cathode-driven reactions that occur during battery operation. With a deeper understanding of the CEI and the processes that lead to its formation, these advanced characterization tools can unlock routes to mitigate impedance rise, particle cracking, transition metal dissolution, and electrolyte consumption, ultimately enabling longer lasting, safer batteries.

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“…In recent years, the application of APT to nanoparticles, [12][13][14] nanowires, [15,16] and nanosheets [17] has triggered a reckoning that the detailed composition and the presence of trace impurities are of paramount importance when it comes to understanding the activity of nanomaterials. [18] Impurity elements in the raw materials used during the synthesis may not react at the same rate and hence be preferentially incorporated into the final product, [17] or may be incorporated into the structure during processing or synthesis by wet chemistry. [19,20] For MXenes and their surface terminations, most studies to date have relied heavily on X-ray (photoelectron) spectroscopy and electron microscopy techniques for compositional measurements.…”

Section: Introductionmentioning

confidence: 99%

Near‐Atomic‐Scale Perspective on the Oxidation of Ti₃C₂T_x MXenes: Insights from Atom Probe Tomography

Krämer,

Favelukis,

El‐Zoka

et al. 2023

Advanced Materials

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MXenes are a family of 2D transition metal carbides and nitrides with remarkable properties and great potential for energy storage and catalysis applications. However, their oxidation behavior is not yet fully understood, and there are still open questions regarding the spatial distribution and precise quantification of surface terminations, intercalated ions, and possible uncontrolled impurities incorporated during synthesis and processing. Here, atom probe tomography analysis of as‐synthesized Ti3C2Tx MXenes reveals the presence of alkali (Li, Na) and halogen (Cl, F) elements as well as unetched Al. Following oxidation of the colloidal solution of MXenes, it is observed that the alkalies enriched in TiO2 nanowires. Although these elements are tolerated through the incorporation by wet chemical synthesis, they are often overlooked when the activity of these materials is considered, particularly during catalytic testing. This work demonstrates how the capability of atom probe tomography to image these elements in 3D at the near‐atomic scale can help to better understand the activity and degradation of MXenes, in order to guide their synthesis for superior functional properties.This article is protected by copyright. All rights reserved

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Atomic-scale characterization of (electro-)catalysts and battery materials by atom probe tomography

Cited by 10 publications

References 76 publications

Facilitating the Systematic Nanoscale Study of Battery Materials by Atom Probe Tomography through in‐situ Metal Coating

Facilitating the Systematic Nanoscale Study of Battery Materials by Atom Probe Tomography through in‐situ Metal Coating

Beyond Composition: Surface Reactivity and Structural Arrangement of the Cathode–Electrolyte Interphase

Near‐Atomic‐Scale Perspective on the Oxidation of Ti₃C₂T_x MXenes: Insights from Atom Probe Tomography

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Atomic-scale characterization of (electro-)catalysts and battery materials by atom probe tomography

Cited by 10 publications

References 76 publications

Facilitating the Systematic Nanoscale Study of Battery Materials by Atom Probe Tomography through in‐situ Metal Coating

Facilitating the Systematic Nanoscale Study of Battery Materials by Atom Probe Tomography through in‐situ Metal Coating

Beyond Composition: Surface Reactivity and Structural Arrangement of the Cathode–Electrolyte Interphase

Near‐Atomic‐Scale Perspective on the Oxidation of Ti3C2Tx MXenes: Insights from Atom Probe Tomography

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Near‐Atomic‐Scale Perspective on the Oxidation of Ti₃C₂T_x MXenes: Insights from Atom Probe Tomography