Novel Method for Preparing Transmission Electron Microscopy Samples of Micrometer-Sized Powder Particles by Using Focused Ion Beam

2017 ◽  
Vol 23 (5) ◽  
pp. 1055-1060 ◽  
Author(s):  
Tae-Hoon Kim ◽  
Min-Chul Kang ◽  
Ga-Bin Jung ◽  
Dong Soo Kim ◽  
Cheol-Woong Yang
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
Size Range ◽  
Ion Beam ◽  
Preparation Technique ◽  
Simple Method ◽  
Transmission Electron ◽  
Powder Particles ◽  
Novel Method

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.

Preparation of TEM Specimens from Gas-Atomized Fe-6.5wt.%Si Powders with Several Micrometers Using Focused Ion Beam

2013 ◽  
Vol 706-708 ◽  
pp. 224-229
Author(s):  
Shi Chao Zhao ◽  
Ke Xie ◽  
Chang Jiang Song ◽  
Qi Jie Zhai
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Electron Diffraction ◽  
Focused Ion Beam ◽  
Preparation Method ◽  
Ion Beam ◽  
Selected Area Electron Diffraction ◽  
Transmission Electron ◽  
Powder Particles ◽  
Novel Method

Transmission electron microscopy (TEM) can be utilized to identify some specific microstructures of metals and alloys. However, it is very difficult to precisely prepare a TEM specimen from the powder particles with several micrometers. There are more or less drawbacks in conventional preparation method. This paper describes a novel method to prepare specific specimens from the powder particles with several micrometers for TEM study. A TEM specimen approximately 5μm diameter was successfully prepared to electron transparency, which extracted from a 5μm diameter powder particle. The selected-area electron diffraction pattern (SAED) analysis was carried out.

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.

Defect Analysis and Process Development of Microelectronics Devices Using Focused Ion Beam and Energy Filtering Transmission Electron Microscopy.

1999 ◽  
Vol 5 (S2) ◽  
pp. 900-901
Author(s):  
R. Pantel ◽  
G. Mascarin ◽  
G. Auvert
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
Process Development ◽  
Ion Beam ◽  
Preparation Technique ◽  
Defect Analysis ◽  
Tem Analysis ◽  
Energy Filtering ◽  
Transmission Electron

1. Introduction.With continuing reductions in semiconductor device dimensions high spatial resolution physical and chemical analysis techniques will be more and more required for defect analysis and process development in the microelectronics field. Transmission Electron Microscopy (TEM) analysis is now extensively used thanks to the fast Focused Ion Beam (FIB) specimen preparation technique which has furthered its development. Recently, we have shown the advantages of adding Electron Energy Loss Spectroscopy (EELS) to FIB-TEM analysis for semiconductor process characterization. In this paper we extend the EELS technique using FIB sample preparation to Energy Filtering TEM (EFTEM) observations. The EFTEM analysis allows high-resolution compositional mapping using spectroscopic imaging of core level ionization edges3. We show some applications of FIB-EFTEM to defect analysis and process development.2. Experimental details.The FIB system is a MICRION model 9500 EX using a gallium ion beam of 50 keV maximum energy with a 5 nm minimum spot diameter.

Characterization of Dislocation Structures in Hexagonal SiC by Transmission Electron Microscopy

2012 ◽  
Vol 725 ◽  
pp. 11-14 ◽  
Author(s):  
Yoshihiro Sugawara ◽  
Y. Yao ◽  
Yukari Ishikawa ◽  
Katsunori Danno ◽  
Hiroshi Suzuki ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Large Angle ◽  
Preparation Technique ◽  
Transmission Electron ◽  
Low Dislocation Density ◽  
Basal Plane Dislocation ◽  
Convergent Beam

We developed the transmission electron microscopy (TEM) sample preparation technique for the low dislocation density of 4H-SiC by combining the KOH+Na2O2 (KN) etching and the focused ion beam (FIB) microsampling technique. The dislocation under sea-shell pit was then characterized by large-angle convergent-beam electron diffraction (LACBED). It is demonstrated that this method is powerful for evaluating Burgers vectors of dislocations. Burgers vector of the measured basal plane dislocation (BPD) is determined to be b=1/3[-12-10]. Two-beam bright-field (TBBF) imaging identified the rotating direction of the threading screw dislocation (TSD) is counter-clockwise.

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.

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