scholarly journals Multi-length Scale Cryogenic Sample Preparation to Electron Microscopy of Battery Materials

2020 ◽  
Vol 26 (S2) ◽  
pp. 3022-3024
Author(s):  
Cecile Bonifacio ◽  
Pawel Nowakowski ◽  
Mary Ray ◽  
Paul Fischione
Author(s):  
Ching Shan Sung ◽  
Hsiu Ting Lee ◽  
Jian Shing Luo

Abstract Transmission electron microscopy (TEM) plays an important role in the structural analysis and characterization of materials for process evaluation and failure analysis in the integrated circuit (IC) industry as device shrinkage continues. It is well known that a high quality TEM sample is one of the keys which enables to facilitate successful TEM analysis. This paper demonstrates a few examples to show the tricks on positioning, protection deposition, sample dicing, and focused ion beam milling of the TEM sample preparation for advanced DRAMs. The micro-structures of the devices and samples architectures were observed by using cross sectional transmission electron microscopy, scanning electron microscopy, and optical microscopy. Following these tricks can help readers to prepare TEM samples with higher quality and efficiency.


Author(s):  
Chin Kai Liu ◽  
Chi Jen. Chen ◽  
Jeh Yan.Chiou ◽  
David Su

Abstract Focused ion beam (FIB) has become a useful tool in the Integrated Circuit (IC) industry, It is playing an important role in Failure Analysis (FA), circuit repair and Transmission Electron Microscopy (TEM) specimen preparation. In particular, preparation of TEM samples using FIB has become popular within the last ten years [1]; the progress in this field is well documented. Given the usefulness of FIB, “Artifact” however is a very sensitive issue in TEM inspections. The ability to identify those artifacts in TEM analysis is an important as to understanding the significance of pictures In this paper, we will describe how to measure the damages introduced by FIB sample preparation and introduce a better way to prevent such kind of artifacts.


2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Bing Han ◽  
Yucheng Zou ◽  
Zhen Zhang ◽  
Xuming Yang ◽  
Xiaobo Shi ◽  
...  

AbstractCryogenic transmission electron microscopy (cryo-TEM) is a valuable tool recently proposed to investigate battery electrodes. Despite being employed for Li-based battery materials, cryo-TEM measurements for Na-based electrochemical energy storage systems are not commonly reported. In particular, elucidating the chemical and morphological behavior of the Na-metal electrode in contact with a non-aqueous liquid electrolyte solution could provide useful insights that may lead to a better understanding of metal cells during operation. Here, using cryo-TEM, we investigate the effect of fluoroethylene carbonate (FEC) additive on the solid electrolyte interphase (SEI) structure of a Na-metal electrode. Without FEC, the NaPF6-containing carbonate-based electrolyte reacts with the metal electrode to produce an unstable SEI, rich in Na2CO3 and Na3PO4, which constantly consumes the sodium reservoir of the cell during cycling. When FEC is used, the Na-metal electrode forms a multilayer SEI structure comprising an outer NaF-rich amorphous phase and an inner Na3PO4 phase. This layered structure stabilizes the SEI and prevents further reactions between the electrolyte and the Na metal.


1992 ◽  
Vol 281 ◽  
Author(s):  
S. Shih ◽  
K. H. Jung ◽  
D. L. Kwong

ABSTRACTWe have developed a new, minimal damage approach for examination of luminescent porous Si layers (PSLs) by transmission electron microscopy (TEM). In this approach, chemically etched PSLs are fabricated after conventional plan-view TEM sample preparation. A diffraction pattern consisting of a diffuse center spot, characteristic of amorphous material, is primarily observed. However, crystalline, microcrystalline, and amorphous regions could all be observed in selected areas. A crystalline mesh structure could be observed in some of the thin areas near the pinhole. The microcrystallite sizes were 15–150 Å and decreased in size when located further from the pinhole.


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