Ultra-Microtome for the Preparation of TEM Specimens from Battery Cathodes

Zhang, Hanlei; Wang, Chongmin; Zhou, Guangwen

doi:10.1017/s1431927620024368

Cited by 10 publications

(17 citation statements)

References 74 publications

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“…To reduce the effects of this carbon-based contamination during electron beam exposure, a plasma cleaning system can be used to remove carbon residue on the epoxy embedded cross sections while supported on the TEM grids. Other ways of minimizing carbon contamination during S/TEM analyses include the use of electron beam irradiation of the sample at current intensities of ∼20 pA nm –2 s –1 prior to imaging . Representative sections of epoxy supporting the cross sections of cathode particles are shown in a series of low- to high-magnification TEM images (Figure S5).…”

Section: Resultsmentioning

confidence: 99%

“…For example, Figure S12 exhibits a well-defined angular edge of a particle with an uneven LiNbO 3 coating. A patch of LiNbO 3 was also formed on one cross section (Figure S14), which could have resulted from the redeposition of a section of LiNbO 3 particles during sample processing . The transfer of cross sections to the TEM grid from the air-water interface of the microtome trough could inadvertently result in the redistribution of loosely adhered material due to the strong surface tension forces.…”

Section: Resultsmentioning

confidence: 99%

“…Other ways of minimizing carbon contamination during S/TEM analyses include the use of electron beam irradiation of the sample at current intensities of ∼20 pA nm −2 s −1 prior to imaging. 13 Representative sections of epoxy supporting the cross sections of cathode particles are shown in a series of low-to high-magnification TEM images (Figure S5). Sharp, angular edges of the sample are exhibited at the higher magnifications and are most representative of an intact particle morphology.…”

Section: Resultsmentioning

confidence: 99%

“…Enabling an efficient, high-throughput characterization of the interface between these coatings and the cathode particle will enable improvements to the design of methods used to prepare and tune the properties of the cathode coatings. The use of an ultramicrotome method for the preparation of cathode specimens has shown promise as an efficient method for atomic-scale characterization . This technique could help to establish a more complete interpretation of both the chemical and physical properties of these interfaces.…”

Section: Introductionmentioning

confidence: 99%

“…The use of an ultramicrotome method for the preparation of cathode specimens has shown promise as an efficient method for atomic-scale characterization. 13 This technique could help to establish a more complete interpretation of both the chemical and physical properties of these interfaces. Bulk particle− surface correlations are required for cathode coating development and could be more easily achieved through an efficient preparation of sample cross sections.…”

Section: Introductionmentioning

confidence: 99%

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Enabling a High-Throughput Characterization of Microscale Interfaces within Coated Cathode Particles

Taylor

Nesvaderani²,

Ovens

et al. 2021

ACS Appl. Energy Mater.

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Lithium-ion batteries represent an emerging field. The development of battery materials could benefit from quick techniques that enable atomic-level diagnostics. High-performance cathodes, such as high-voltage spinel, often require coatings to protect against the destructive electrochemical environments at the particle–electrolyte interface. The preparations of these coatings are still in the early phases of development, and their analytical inspection by high-resolution scanning and transmission electron microscopy (HR-S/TEM) techniques presents a significant challenge due to the microscale dimensions of the cathode particles. In this work, a high-throughput ultramicrotome technique was assessed for the characterization of the particle–coating interface. The ultramicrotome technique enabled the rapid preparation of cross sections with a thickness of 126 ± 66 nm as determined by electron energy loss spectroscopy (EELS) measurements. Cathode particles composed of high-voltage spinel, LiNi0.5Mn1.5O4 (LNMO), coated with lithium niobate (LiNbO3) were synthesized, and cross sections were inspected using HR-S/TEM techniques. These ultrathin cross sections enabled the ability to obtain nanoscale information regarding the composition and crystallinity of the particle–coating interface over lateral areas of >1 μm. Accessible correlations between the electrochemical performance of the LiNbO3-coated LNMO particles and the HR-S/TEM results were enabled by the high-throughput method. Discharge capacity measurements were acquired over a series of 100 electrochemical cycles for both the LiNbO3 coated and the as-prepared LNMO particles. The limitations of the ultramicrotome technique are also discussed herein with respect to the coating morphology and the procedure for guidance toward technique optimization. The rapid preparation of ultrathin cross sections can assist the advancement of protective coatings on the surfaces of cathode particles for an efficient characterization of bulk–surface interfaces.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Enabling a High-Throughput Characterization of Microscale Interfaces within Coated Cathode Particles

Taylor

Nesvaderani²,

Ovens

et al. 2021

ACS Appl. Energy Mater.

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Oxygen Loss in Layered Oxide Cathodes for Li-Ion Batteries: Mechanisms, Effects, and Mitigation

et al. 2022

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Layered lithium transition metal oxides derived from LiMO 2 (M = Co, Ni, Mn, etc.) have been widely adopted as the cathodes of Li-ion batteries for portable electronics, electric vehicles, and energy storage. Oxygen loss in the layered oxides is one of the major factors leading to cycling-induced structural degradation and its associated fade in electrochemical performance. Herein, we review recent progress in understanding the phenomena of oxygen loss and the resulting structural degradation in layered oxide cathodes. We first present the major driving forces leading to the oxygen loss and then describe the associated structural degradation resulting from the oxygen loss. We follow this analysis with a discussion of the kinetic pathways that enable oxygen loss, and then we address the resulting electrochemical fade. Finally, we review the possible approaches toward mitigating oxygen loss and the associated electrochemical fade as well as detail novel analytical methods for probing the oxygen loss.

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Revealing the 3D Structure of Block Copolymers with Electron Microscopy: Current Status and Future Directions

Weisbord

Segal‐Peretz

2023

ACS Appl. Mater. Interfaces

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Block copolymers (BCPs) are considered model systems for understanding and utilizing self-assembly in soft matter. Their tunable nanometric structure and composition enable comprehensive studies of self-assembly processes as well as make them relevant materials in diverse applications. A key step in developing and controlling BCP nanostructures is a full understanding of their three-dimensional (3D) structure and how this structure is affected by the BCP chemistry, confinement, boundary conditions, and the self-assembly evolution and dynamics. Electron microscopy (EM) is a leading method in BCP 3D characterization owing to its high resolution in imaging nanosized structures. Here we discuss the two main 3D EM methods: namely, transmission EM tomography and slice and view scanning EM tomography. We present each method’s principles, examine their strengths and weaknesses, and discuss ways researchers have devised to overcome some of the challenges in BCP 3D characterization with EM- from specimen preparation to imaging radiation-sensitive materials. Importantly, we review current and new cutting-edge EM methods such as direct electron detectors, energy dispersive X-ray spectroscopy of soft matter, high temporal rate imaging, and single-particle analysis that have great potential for expanding the BCP understanding through EM in the future.

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Ultra-Microtome for the Preparation of TEM Specimens from Battery Cathodes

Abstract: Abstract

Cited by 10 publications

References 74 publications

Enabling a High-Throughput Characterization of Microscale Interfaces within Coated Cathode Particles

Enabling a High-Throughput Characterization of Microscale Interfaces within Coated Cathode Particles

Oxygen Loss in Layered Oxide Cathodes for Li-Ion Batteries: Mechanisms, Effects, and Mitigation

Revealing the 3D Structure of Block Copolymers with Electron Microscopy: Current Status and Future Directions

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