Effect of nanosectioning on surface features and stiffness of an amorphous glassy polymer

Sun, Fengzhen; Li, Hu; Leifer, Klaus; Gamstedt, E. Kristofer

doi:10.1002/pen.24793

Cited by 3 publications

(1 citation statement)

References 41 publications

(78 reference statements)

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“…Certain speeds could result in mechanical damage. Previous studies have investigated the effects of shear forces induced by the influences of changes in the sectioning speed on poly(methyl methacrylate) or PMMA. , Sections of PMMA prepared at relatively high sectioning speeds of 1.0 mm/s exhibited regular shear deformations with morphologies similar to those observed in the fractured sections of cathode particles (Figure S16). This correlation suggests that the sectioning speed for an amorphous polymer should be as slow as possible for minimizing the defects introduced from this strain.…”

Section: Resultsmentioning

confidence: 86%

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: 86%

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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Repetitive ultramicrotome trimming and SEM imaging for characterizing printed multilayer structures

Huang,

Mach,

Binder

et al. 2024

Sci Rep

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Ultramicrotomy is a well-established technique that has been applied in biology and medical research to produce thin sections or a blockface of an embedded sample for microscopy. Recently, this technique has also been applied in materials science or micro- and nanotechnology as a sample preparation method for subsequent characterization. In this work, an application of ultramicrotomy for the cross-section preparation of an inkjet-printed multilayer structure is demonstrated. The investigated device is a capacitor consisting of three layers. The top and bottom electrodes are printed with silver nanoparticle ink and the dielectric layer with a ceramic nanoparticle/polymer ink. A 3D profilometer is initially used to study the surface morphology of the printed multilayer. The measurements show that both electrodes exhibit a coffee-ring effect, which results in an inhomogeneous layer structure of the device. To obtain precise 3D information on the multilayer, cross-sections must be prepared. Argon ion beam milling is the current gold standard to produce a single cross-section in good quality, however, the cross-section position within the multilayer volume is poorly defined. Moreover, the milling process requires a significant investment of time and resources. Herein, we develop an efficient method to realize repetitive cross-section preparation at well-defined positions in the multilayer volume. Repetitive cross-sections are exposed by trimming with an ultramicrotome (UM) and this blockface is subsequently transferred into a scanning electron microscope (SEM) for imaging. A combination of custom-modified UM and SEM specimen holders allows repeated transfer of the clamped multilayer sample between instruments without damage and with high positioning accuracy. This novel approach enhances the combination of an established ultramicrotome and a SEM for multilayer sample volume investigation. Thus, a comprehensive understanding of printed multilayer structures can be gained, to derive insights for optimization of device architecture and printing process.

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Direct measurement of the surface energy of single-walled carbon nanotubes through atomic force microscopy

Liu

Papadakis

2019

Journal of Applied Physics

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Surface energy in nanomaterials is an essential parameter demonstrating a key role in their surface interactions and their functionalization aptitude. In this work, a new and facile methodology based on atomic force microscopy for the measurement of the surface energy of single-walled carbon nanotubes (SWCNTs) is reported. The proposed approach starts with the calibration based on a well-studied material, graphite, and the precision of the technique is confirmed by the measurement of the surface energy of multiwalled carbon nanotubes. Our measurements show that SWCNTs display a surface energy of 52.8 mJ/m2, which is in very good agreement with theoretical predictions of the measured property. Our experimental approach is essentially applicable to other nano-objects in contrast to conventional wet angle methods which are currently employed mainly in bulk materials.

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Effect of nanosectioning on surface features and stiffness of an amorphous glassy polymer

Cited by 3 publications

References 41 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

Repetitive ultramicrotome trimming and SEM imaging for characterizing printed multilayer structures

Direct measurement of the surface energy of single-walled carbon nanotubes through atomic force microscopy

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