scholarly journals Sample Preparation Methodologies for In Situ Liquid and Gaseous Cell Analytical Transmission Electron Microscopy of Electropolished Specimens

2016 ◽  
Vol 22 (6) ◽  
pp. 1350-1359 ◽  
Author(s):  
Xiang Li Zhong ◽  
Sibylle Schilling ◽  
Nestor J. Zaluzec ◽  
M. Grace Burke
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
General Procedure ◽  
Ion Beam ◽  
Metals And Alloys ◽  
Stainless Steel Sample ◽  
Transmission Electron ◽  
Wide Range

AbstractIn recent years, an increasing number of studies utilizing in situ liquid and/or gaseous cell scanning/transmission electron microscopy (S/TEM) have been reported. Because of the difficulty in the preparation of suitable specimens, these environmental S/TEM studies have been generally limited to studies of nanoscale structured materials such as nanoparticles, nanowires, or sputtered thin films. In this paper, we present two methodologies which have been developed to facilitate the preparation of electron-transparent samples from conventional bulk metals and alloys for in situ liquid/gaseous cell S/TEM experiments. These methods take advantage of combining sequential electrochemical jet polishing followed by focused ion beam extraction techniques to create large electron-transparent areas for site-specific observation. As an example, we illustrate the application of this methodology for the preparation of in situ specimens from a cold-rolled Type 304 austenitic stainless steel sample, which was subsequently examined in both 1 atm of air as well as fully immersed in a H2O environment in the S/TEM followed by hyperspectral imaging. These preparation techniques can be successfully applied as a general procedure for a wide range of metals and alloys, and are suitable for a variety of in situ analytical S/TEM studies in both aqueous and gaseous environments.

scholarly journals In Situ Preparation of Pr1-xCaxMnO3 and La1-xSrxMnO3 Catalysts Surface for High-Resolution Environmental Transmission Electron Microscopy

Catalysts ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 751 ◽  
Author(s):  
Roddatis ◽  
Lole ◽  
Jooss
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Residual Water ◽  
Environmental Transmission ◽  
Transmission Electron ◽  
Environmental Transmission Electron Microscopy

The study of changes in the atomic structure of a catalyst under chemical reaction conditions is extremely important for understanding the mechanism of their operation. For in situ environmental transmission electron microscopy (ETEM) studies, this requires preparation of electron transparent ultrathin TEM lamella without surface damage. Here, thin films of Pr1-xCaxMnO3 (PCMO, x = 0.1, 0.33) and La1-xSrxMnO3 (LSMO, x = 0.4) perovskites are used to demonstrate a cross-section specimen preparation method, comprised of two steps. The first step is based on optimized focused ion beam cutting procedures using a photoresist protection layer, finally being removed by plasma-etching. The second step is applicable for materials susceptible to surface amorphization, where in situ recrystallization back to perovskite structure is achieved by using electron beam driven chemistry in gases. This requires reduction of residual water vapor in a TEM column. Depending on the gas environment, long crystalline facets having different atomic terminations and Mn-valence state, can be prepared.

scholarly journals Fabrication of a Lift-Out Grid with Electrical Contacts for Focused Ion Beam Preparation of Lamella for In Situ Transmission Electron Microscopy

2013 ◽  
Vol 19 (S2) ◽  
pp. 458-459 ◽  
Author(s):  
M. Mecklenburg ◽  
M. Brodie ◽  
W. Hubbard ◽  
E.R. White ◽  
A. Bushmaker ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Electrical Contacts ◽  
Transmission Electron

Extended abstract of a paper presented at Microscopy and Microanalysis 2013 in Indianapolis, Indiana, USA, August 4 – August 8, 2013.

Applications of Ion Microscopy and In Situ Electron Microscopy to the Study of Electronic Materials and Devices

1998 ◽  
Vol 4 (3) ◽  
pp. 308-316 ◽  
Author(s):  
R. Hull ◽  
J. Demarest ◽  
D. Dunn ◽  
E.A. Stach ◽  
Q. Yuan
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
Electronic Materials ◽  
Ion Beam ◽  
Microscopy Imaging ◽  
Transmission Electron ◽  
In Situ Electron Microscopy ◽  
Ion Microscopy

We discuss the application of ion microscopy and in situ electron microscopy to the study of electronic and optical materials and devices. We demonstrate how the combination of in situ transmission electron microscopy and focused ion beam microscopy provides new avenues for the study for such structures, enabling extension of these techniques to the study of dopant distributions, nanoscale stresses, three-dimensional structural and chemical reconstruction, and real-time evolution of defect microstructure. We also discuss in situ applications of thermal, mechanical, electrical, and optical stresses during transmission electron microscopy imaging.

Recent Advances in FIB Technology for Nano-prototyping and Nano-characterisation

2007 ◽  
Vol 1020 ◽  
Author(s):  
Debbie J Stokes ◽  
Laurent Roussel ◽  
Oliver Wilhelmi ◽  
Lucille A Giannuzzi ◽  
Dominique HW Hubert
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Scanning Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Nano Materials ◽  
Transmission Electron ◽  
Scanning Transmission

AbstractCombined focused ion beam (FIB) and scanning electron microscopy (SEM) methods are becoming increasingly important for nano-materials applications as we continue to develop ways to exploit the complex interplay between primary ion and electron beams and the substrate, in addition to the various subtle relationships with gaseous intermediaries.We demonstrate some of the recent progress that has been made concerning FIB SEM processing of both conductive and insulating materials for state-of-the-art nanofabrication and prototyping and superior-quality specimen preparation for ultra-high resolution scanning transmission electron microscopy (STEM) and transmission electron microscopy (TEM) imaging and related in situ nanoanalysis techniques.

Cross-Sectional Transmission Electron Microscopy Sample Preparation Using Focus Ion Beam Machine and Wedge Technique

1999 ◽  
Vol 5 (S2) ◽  
pp. 894-895 ◽  
Author(s):  
Du Li ◽  
Rose Zhou ◽  
Rob Zanoya
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
General Procedure ◽  
Ion Beam ◽  
Optical Microscope ◽  
Cross Sectional ◽  
Transmission Electron ◽  
Focus Ion Beam ◽  
Tem Grid

As features on an IC chip become smaller than the resolution power of an optical microscope and of the size of the grinding particles, the trend for preparing cross-sectional transmission electron microscopy (TEM) samples at specific locations (bits) is moving towards using a focused ion beam (FIB) machine. Details on how to use a FIB machine to prepare cross-sectional TEM samples have been outlined in many references.The general procedure is to first mark the specific location (bit) in the FIB machine and then grind the sample down to about 20 microns, 10 microns on each side of the feature of interest. After grinding, the sample is mounted on a pre-cut TEM grid and thinned with the FIB to about 0.1 micron in the region containing the feature of interest. There are several disadvantages to this method. First, the sample goes into the FIB machine at least twice—once for FIB marks on the location and once again for the final thinning.

Design and Application of a Novel In Situ Nano-Manipulation Stage for Transmission Electron Microscopy

2015 ◽  
Vol 21 (2) ◽  
pp. 298-306 ◽  
Author(s):  
Bon-Woong Koo ◽  
Seung-Pyo Hong ◽  
Seong-Il Kim ◽  
Chan S. Kang ◽  
Sang-Sub Han ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
Electrochemical Etching ◽  
Ion Beam ◽  
Pearlitic Steel ◽  
Silver Nanowire ◽  
Nano Scale ◽  
Transmission Electron

AbstractA novel nano-scale manipulator capable of handling low-dimensional materials with three-dimensional linear motion, gripping action, and push–pull action of the gripper was developed for an in situ experiment in transmission electron microscopy. X-Y-Z positioning and push–pull action were accomplished by a piezotubing system, combined with a specially designed assembly stage that consisted of a lever-action gripping tip backed by a push–pull piezostack. The gripper tip consisted of tungsten wire fabricated by electrochemical etching followed by a focused ion beam process. Performance of the nano-scale manipulator was demonstrated in a grab-and-pick test of a single silver nanowire and in an in situ tensile test of a pearlitic steel sample with a specific orientation.

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