Atom probe analysis of BaTiO3 enabled by metallic shielding

Kim, Se‐Ho; Shin, Kihyun; Zhou, Xuyang; Jung, Chanwon; Kim, Hyun You; Pedrazzini, S.; Conroy, Michele; Henkelman, Graeme; Gault, Baptiste

doi:10.1016/j.scriptamat.2023.115370

Cited by 4 publications

(2 citation statements)

References 42 publications

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“…[22][23][24] Coating have also been used for improved analytical performance, as reported by, e. g., Larson et al [25] and Seol et al, [26] who demonstrated improvement in mass resolving power through reduction in thermal tails from laser pulsing. In another study, Kim et al [27] embedded BaTiO 3 , a perovskite-structured material, into a nickel matrix. Application of the metallic coating effectively prevented charge penetration caused by the electrostatic field and enabled the APT analysis.…”

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%

“…and Seol et al., [26] who demonstrated improvement in mass resolving power through reduction in thermal tails from laser pulsing. In another study, Kim et al [27] . embedded BaTiO 3 , a perovskite‐structured material, into a nickel matrix.…”

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

Self Cite

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Direct Observation of Trace Elements in Barium Titanate of Multilayer Ceramic Capacitors Using Atom Probe Tomography

Jang,

Kim,

Jung

et al. 2024

Microscopy and Microanalysis

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Accurately controlling trace additives in dielectric barium titanate (BaTiO3) layers is important for optimizing the performance of multilayer ceramic capacitors (MLCCs). However, characterizing the spatial distribution and local concentration of the additives, which strongly influence the MLCC performance, poses a significant challenge. Atom probe tomography (APT) is an ideal technique for obtaining this information, but the extremely low electrical conductivity and piezoelectricity of BaTiO3 render its analysis with existing sample preparation approaches difficult. In this study, we developed a new APT sample preparation method involving W coating and heat treatment to investigate the trace additives in the BaTiO3 layer of MLCCs. This method enables determination of the local concentration and distribution of all trace elements in the BaTiO3 layer, including additives and undesired impurities. The developed method is expected to pave the way for the further optimization and advancement of MLCC technology.

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Facilitating Atom Probe Tomography of 2D MXene Films by In Situ Sputtering

Krämer,

Favelukis,

Sokol

et al. 2024

Microscopy and Microanalysis

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2D materials are emerging as promising nanomaterials for applications in energy storage and catalysis. In the wet chemical synthesis of MXenes, these 2D transition metal carbides and nitrides are terminated with a variety of functional groups, and cations such as Li+ are often used to intercalate into the structure to obtain exfoliated nanosheets. Given the various elements involved in their synthesis, it is crucial to determine the detailed chemical composition of the final product, in order to better assess and understand the relationships between composition and properties of these materials. To facilitate atom probe tomography analysis of these materials, a revised specimen preparation method is presented in this study. A colloidal Ti3C2Tz MXene solution was processed into an additive-free free-standing film and specimens were prepared using a dual beam scanning electron microscope/focused ion beam. To mechanically stabilize the fragile specimens, they were coated using an in situ sputtering technique. As various 2D material inks can be processed into such free-standing films, the presented approach is pivotal for enabling atom probe analysis of other 2D materials.

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Atom probe analysis of BaTiO3 enabled by metallic shielding

Cited by 4 publications

References 42 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

Direct Observation of Trace Elements in Barium Titanate of Multilayer Ceramic Capacitors Using Atom Probe Tomography

Facilitating Atom Probe Tomography of 2D MXene Films by In Situ Sputtering

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