scholarly journals TEM sample preparation for Li-ion secondary battery using ion slicer

2021 ◽  
Author(s):  
JungSik Park ◽  
Yoon-Jung Kang ◽  
SunEui Choi ◽  
YongNam Jo
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Spherical Aberration ◽  
Lithium Ion ◽  
Ion Milling ◽  
Intrinsic Structure ◽  
Tem Analysis ◽  
Secondary Battery ◽  
Transmission Electron

Abstract The main purpose in this paper is a sample preparation of transmission electron microscopy (TEM) for the lithium-ion secondary battery in the form of micro-sized powders. To avoid artefacts of the TEM sample preparation, the use of ion slicer milling for thinning and maintaining the intrinsic structure is described. Argon-ion milling techniques have been widely examined to make the optimized specimen, which makes TEM analysis more reliable. In the past few years, the correction of spherical aberration (Cs) in scanning transmission electron microscopy (STEM) has been developing rapidly, that results in the direct observation with the atomic level resolution not only for the high acceleration voltage but also its deaccelerated voltage as well. Especially, low-kV application has been markedly increased that needs the sufficient-transparent specimen without the structural distortion during the process of the sample preparation. In this study, the sample preparation for the high-resolution STEM observation has been greatly accomplished and investigations of its crystal integrity are carried out by Cs-corrected STEM.

scholarly journals TEM sample preparation of microsized LiMn2O4 powder using an ion slicer

2021 ◽  
Vol 51 (1) ◽  
Author(s):  
Jung Sik Park ◽  
Yoon-Jung Kang ◽  
Sun Eui Choi ◽  
Yong Nam Jo
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Spherical Aberration ◽  
Lithium Ion ◽  
Ion Milling ◽  
Intrinsic Structure ◽  
Tem Analysis ◽  
Transmission Electron ◽  
Scanning Transmission

AbstractThe main purpose of this paper is the preparation of transmission electron microscopy (TEM) samples from the microsized powders of lithium-ion secondary batteries. To avoid artefacts during TEM sample preparation, the use of ion slicer milling for thinning and maintaining the intrinsic structure is described. Argon-ion milling techniques have been widely examined to make optimal specimens, thereby making TEM analysis more reliable. In the past few years, the correction of spherical aberration (Cs) in scanning transmission electron microscopy (STEM) has been developing rapidly, which results in direct observation at an atomic level resolution not only at a high acceleration voltage but also at a deaccelerated voltage. In particular, low-kV application has markedly increased, which requires a sufficiently transparent specimen without structural distortion during the sample preparation process. In this study, sample preparation for high-resolution STEM observation is accomplished, and investigations on the crystal integrity are carried out by Cs-corrected STEM.

TEM Sample Preparation Tricks for Advanced DRAMs

2015 ◽  
Author(s):  
Ching Shan Sung ◽  
Hsiu Ting Lee ◽  
Jian Shing Luo
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Integrated Circuit ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Tem Analysis ◽  
Cross Sectional ◽  
Transmission Electron ◽  
Characterization Of Materials

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.

A Methodology to Reduce Ion Beam Induced Damage in TEM Specimens Prepared by FIB

2002 ◽  
Author(s):  
Chin Kai Liu ◽  
Chi Jen. Chen ◽  
Jeh Yan.Chiou ◽  
David Su
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Integrated Circuit ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Tem Analysis ◽  
Sensitive Issue ◽  
Transmission Electron

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.

Improving transmission electron microscopy characterization of semiconductors by minimizing sample preparation artifacts

1992 ◽  
Vol 70 (10-11) ◽  
pp. 875-880 ◽  
Author(s):  
J. P. McCaffrey ◽  
G. I. Sproule ◽  
R. Sargent
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Ion Milling ◽  
Transmission Electron ◽  
Transmission Electron Microscopy Characterization ◽  
Silicon Based ◽  
Microscopy Characterization ◽  
Preparation Techniques

Techniques employed for the preparation of transmission electron microscopy (TEM) samples can introduce artifacts that obscure subtle detail in the materials being studied. Traditional semiconductor sample preparation techniques rely heavily on ion milling, which leaves amorphous layers on ion milled surfaces and some intermixing across interfaces, thus degrading the TEM images of these samples. Experimental results of the extent of this amorphization and intermixing are presented for silicon-based semiconductor samples, and methods to minimize these effects are suggested. These methods include variations in ion milling parameters that reduce the extent of the artifacts, and improvements in the small-angle cleavage technique that eliminate these artifacts completely.

Novel Sample Preparation Methods for Transmission Electron Microscopy Observation of Dopant Profiles in Silicon Devices

1999 ◽  
Vol 5 (S2) ◽  
pp. 916-917
Author(s):  
Salvatore Pannitteri
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Ion Milling ◽  
Final Thickness ◽  
Cross Sectional ◽  
Silicon Devices ◽  
First Case ◽  
Transmission Electron ◽  
Dopant Profiles

I present details of novel sample preparation techniques used for delineating two-dimensional dopant profiles in silicon devices. These techniques are based on selective chemical etch of doped silicon in a mixture of hydrofluoric and nitric acid, or simply in buffered HF. The altered topography of the etched surface is imaged by transmission electron microscopy (TEM). Two different strategies will be presented by focusing on their sensitive, resolution, and field of application.In the first case the silicon device is subjected to the conventional thinning procedure for TEM observations in cross-sectional configuration. The final thickness is obtained by Ar ion milling and it can vary between 50 to 500 nm. Sample is then immersed in a chemical solution containing HF (40%), HN03 (65%), and CH3COOH (95%) in the ratio 1:10:10. In presence of an intense illumination this mixture preferentially etches those device regions which are doped with boron, while in order to delineate n-type regions, the etching procedure must be performed in the dark.

The Focused Ion Beam Fold-Out: Sample Preparation Method for Transmission Electron Microscopy

2009 ◽  
Vol 15 (6) ◽  
pp. 558-563 ◽  
Author(s):  
Herman Carlo Floresca ◽  
Jangbae Jeon ◽  
Jinguo G. Wang ◽  
Moon J. Kim
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Ion Milling ◽  
Plan View ◽  
Site Specific ◽  
Area Of Interest ◽  
Transmission Electron

AbstractWe have developed the focused ion beam (FIB) fold-out technique, for transmission electron microscopy (TEM) sample preparation in which there is no fine polishing or dimpling, thus saving turnaround time. It does not require a nanomanipulator yet is still site specific. The sample wafer is cut to shape, polished down, and then placed in a FIB system. A tab containing the area of interest is created by ion milling and then “folded out” from the bulk sample. This method also allows a plan-view of the sample by removing material below the wafer's surface film or device near the polished edge. In the final step, the sample is thinned to electron transparency, ready to be analyzed in the TEM. With both a cross section and plan-view, our technique gives microscopists a powerful tool in analyzing multiple zone axes in one TEM session. The nature of the polished sample edge also includes the ability to sample many areas, allowing the user to examine a very large device or sample. More importantly, this technique could make multiple site-specific e-beam transparent specimens in one polished sample, which is difficult to do when prepared by other methods.

Techniques for Transmission Electron Microscopy of Fiber-Matrix Interfaces in Aluminum Alloy-Boron Composites by Ion Erosio

1971 ◽  
Vol 29 ◽  
pp. 204-205
Author(s):  
G. G. Shaw
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Aluminum Alloy ◽  
Electron Beam ◽  
Pure Aluminum ◽  
Ion Milling ◽  
Transmission Electron ◽  
Fiber Matrix ◽  
Ion Erosion ◽  
Row Of Fibers

The morphology and composition of the fiber-matrix interface can best be studied by transmission electron microscopy and electron diffraction. For some composites satisfactory samples can be prepared by electropolishing. For others such as aluminum alloy-boron composites ion erosion is necessary.When one wishes to examine a specimen with the electron beam perpendicular to the fiber, preparation is as follows: A 1/8 in. disk is cut from the sample with a cylindrical tool by spark machining. Thin slices, 5 mils thick, containing one row of fibers, are then, spark-machined from the disk. After spark machining, the slice is carefully polished with diamond paste until the row of fibers is exposed on each side, as shown in Figure 1.In the case where examination is desired with the electron beam parallel to the fiber, preparation is as follows: Experimental composites are usually 50 mils or less in thickness so an auxiliary holder is necessary during ion milling and for easy transfer to the electron microscope. This holder is pure aluminum sheet, 3 mils thick.

Comparative Microstructures of Ion Milled and Electrochemically Thinned Composite Materials

1974 ◽  
Vol 32 ◽  
pp. 546-547
Author(s):  
R.R. Russell
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Composite Materials ◽  
Great Difficulty ◽  
Ion Milling ◽  
Transmission Electron ◽  
Ion Damage ◽  
Intermetallic Composite

Transmission electron microscopy of metallic/intermetallic composite materials is most challenging since the microscopist typically has great difficulty preparing specimens with uniform electron thin areas in adjacent phases. The application of ion milling for thinning foils from such materials has been quite effective. Although composite specimens prepared by ion milling have yielded much microstructural information, this technique has some inherent drawbacks such as the possible generation of ion damage near sample surfaces.

Transmission Electron Microscopy of an Aluminum-Silver-Stainless Steel Solid State Bond

1985 ◽  
Vol 43 ◽  
pp. 172-173
Author(s):  
M. J. Carr ◽  
J. F. Shewbridge ◽  
T. O. Wilford
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Solid State ◽  
Specimen Preparation ◽  
Dimensional Control ◽  
Tem Analysis ◽  
Metal Parts ◽  
Dissimilar Metal ◽  
Transmission Electron ◽  
Short Time

Strong solid state bonds are routinely produced between physical vapor deposited (PVD) silver coatings deposited on sputter cleaned surfaces of two dissimilar metal parts. The low temperature (200°C) and short time (10 min) used in the bonding cycle are advantageous from the standpoint of productivity and dimensional control. These conditions unfortunately produce no microstructural changes at or near the interface that are detectable by optical, SEM, or microprobe examination. Microstructural problems arising at these interfaces could therefore easily go undetected by these techniques. TEM analysis has not been previously applied to this problem because of the difficulty in specimen preparation. The purpose of this paper is to describe our technique for preparing specimens from solid state bonds and to present our initial observations of the microstructural details of such bonds.

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