Proposals for exact-point transmission-electron microscopy using focused ion beam specimen-preparation technique

Author(s):  
T. Ishitani
Author(s):  
K. Doong ◽  
J.-M. Fu ◽  
Y.-C. Huang

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.


2007 ◽  
Vol 13 (2) ◽  
pp. 80-86 ◽  
Author(s):  
Sara Bals ◽  
Wim Tirry ◽  
Remco Geurts ◽  
Zhiqing Yang ◽  
Dominique Schryvers

Focused ion beam specimen preparation has been used for NiTi samples and SrTiO3/SrRuO3 multilayers with prevention of surface amorphization and Ga implantation by a 2-kV cleaning procedure. Transmission electron microscopy techniques show that the samples are of high quality with a controlled thickness over large scales. Furthermore, preferential thinning effects in multicompounds are avoided, which is important when analytical transmission electron microscopy measurements need to be interpreted in a quantitative manner. The results are compared to similar measurements acquired for samples obtained using conventional preparation techniques such as electropolishing for alloys and ion milling for oxides.


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.


Catalysts ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 751 ◽  
Author(s):  
Roddatis ◽  
Lole ◽  
Jooss

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.


2017 ◽  
Vol 23 (5) ◽  
pp. 1055-1060 ◽  
Author(s):  
Tae-Hoon Kim ◽  
Min-Chul Kang ◽  
Ga-Bin Jung ◽  
Dong Soo Kim ◽  
Cheol-Woong Yang

AbstractThe preparation of transmission electron microscopy (TEM) samples from powders is quite difficult and challenging. For powders with particles in the 1–5 μm size range, it is especially difficult to select an adequate sample preparation technique. Epoxy is commonly used to bind powder, but drawbacks, such as differential milling originating from unequal milling rates between the epoxy and powder, remain. We propose a new, simple method for preparing TEM samples. This method is especially useful for powders with particles in the 1–5 μm size range that are vulnerable to oxidation. The method uses solder as an embedding agent together with focused ion beam (FIB) milling. The powder was embedded in low-temperature solder using a conventional hot-mounting instrument. Subsequently, FIB was used to fabricate thin TEM samples via the lift-out technique. The solder proved to be more effective than epoxy in producing thin TEM samples with large areas. The problem of differential milling was mitigated, and the solder binder was more stable than epoxy under an electron beam. This methodology can be applied for preparing TEM samples from various powders that are either vulnerable to oxidation or composed of high atomic number elements.


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