Site Specific TEM Specimen Preparation using an FIB/TEM System

2000 ◽  
Vol 6 (S2) ◽  
pp. 510-511 ◽  
Author(s):  
T. Kamino ◽  
T. Yaguchi ◽  
T. Ohnishi ◽  
K. Umemura ◽  
S. Tomimatsu
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Site Specific ◽  
Specimen Holder ◽  
Transmission Electron ◽  
Wide Range ◽  
Scanning Transmission

The focused ion beam(FIB) technique, developed for the microelectronics industry has become a major method for site specific transmission electron microscopy(TEM) specimen preparation in a wide range of materials[l]. The FIB lift-out technique has improved the specimen preparation procedures by removing complicated initial fabrication required prior to the FIB milling[2]. However, conventional FIB techniques are still having increased difficulty in meeting failure analysis needs from high technology industries such as microelectronics.We have developed a site specific TEM specimen preparation method using a combination of an FIB instrument and an intermediate voltage TEM equipped with a scanning attachment [3]. In this method, the specimen is mounted on an FIB-TEM compatible specimen holder, so that localization of the specific site can be carried out in the FIB and TEM using the same holder. The scanning electron imaging mode may be used to observe surface structures of the milled area, and the scanning transmission electron microscopy(STEM) mode may be used to observe structures inside of the milled surface.

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.

Focused Ion Beam Milling for Site Specific Scanning and Transmission Electron Microscopy Specimen Preparation

1997 ◽  
Vol 3 (S2) ◽  
pp. 347-348
Author(s):  
L.A. Giannuzzi ◽  
J.L. Drownt ◽  
S.R. Brown ◽  
R.B. Irwin ◽  
F.A. Stevie
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Region Of Interest ◽  
Beam Current ◽  
Specimen Preparation ◽  
Site Specific ◽  
Sem Image ◽  
Transmission Electron

It has been shown that a focused ion beam (FIB) instrument may be used to prepare site specific cross-sectioned specimens to within < 0.1 μm for both scanning and transmission electron microscopy (SEM and TEM, respectively). FIB specimen preparation has been used almost exclusively in the microelectronics industry. Recently, FIB specimen preparation has been utilized for other materials systems and applications.A cross-sectioned SEM specimen is produced by sputtering away a trench of material from near the region of interest. Large amounts of material are sputtered using large ion beam diameters (e.g., l00’s nm) and high beam current (e.g., l000’s pA), while the final sputtering operations are achieved using smaller beam diameters (e.g., < 10 nm) and lower beam current (e.g., 10’s of pA). The SEM specimen may then be etched to reveal particular microstructural features of interest. A low magnification SEM image of a multi-layered device prepared for cross-section analysis by the FIB method is shown in FIG. 1.

Transmission Electron Microscopy (TEM) Specimen Preparation Technique using Focused Ion Beam (FIB): Application to Material Characterization of Chemical Vapor Deposition of Tungsten (W) and Tungsten Silicides (WSix)

1997 ◽  
Author(s):  
K. Doong ◽  
J.-M. Fu ◽  
Y.-C. Huang
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Chemical Vapor Deposition ◽  
Vapor Deposition ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Chemical Vapor ◽  
Specimen Preparation ◽  
Preparation Technique ◽  
Transmission Electron

Abstract The specimen preparation technique using focused ion beam (FIB) to generate cross-sectional transmission electron microscopy (XTEM) samples of chemical vapor deposition (CVD) of Tungsten-plug (W-plug) and Tungsten Silicides (WSix) was studied. Using the combination method including two axes tilting[l], gas enhanced focused ion beam milling[2] and sacrificial metal coating on both sides of electron transmission membrane[3], it was possible to prepare a sample with minimal thickness (less than 1000 A) to get high spatial resolution in TEM observation. Based on this novel thinning technique, some applications such as XTEM observation of W-plug with different aspect ratio (I - 6), and the grain structure of CVD W-plug and CVD WSix were done. Also the problems and artifacts of XTEM sample preparation of high Z-factor material such as CVD W-plug and CVD WSix were given and the ways to avoid or minimize them were suggested.

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.

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.

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