Analysis of the Intermetallic Compound Formed in Hot Dip Aluminized Steel

2006 ◽  
Vol 15-17 ◽  
pp. 159-163 ◽  
Author(s):  
Kee Hyun Kim ◽  
Benny van Daele ◽  
Gustaaf Van Tendeloo ◽  
Yong Sug Chung ◽  
Jong Kyu Yoon

A hot dip aluminising process was carried out with a 1mm steel sheet dipped into the Al-10at.% Si melt in an automatic hot-dip simulator. When steel and liquid aluminium are in contact with each other, a thin intermetallic compound (IMC) is formed between the steel and the aluminium. The analysis and identification of the formation mechanism of the IMC is needed to manufacture the application products. Energy dispersive X-ray spectroscopy (EDX) and electron probe microanalysis (EPMA) are normally used to identify the phases of IMC. In the Al-Fe-Si system, numerous compounds with only slight differences in composition are formed. Consequently, EDX and EPMA are insufficient to confirm exactly the thin IMC with multiphases. In this study, transmission electron microscopy (TEM) analysis combined with EDX was used. The TEM sample was prepared with focused ion beam (FIB) sampling. The FIB lift-out technology is used to slice a very thin specimen with minimum contamination for TEM analysis. It is clearly shown that the IMC consists of Al-27 at. % Fe-10 at. % Si and is identified as Al8Fe2Si with a hexagonal unit cell (space group P63/mmc). The cell parameters are a= 1.2404nm and c= 2.6234nm.

Author(s):  
Ching Shan Sung ◽  
Hsiu Ting Lee ◽  
Jian Shing Luo

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.


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.


Author(s):  
T. Yaguchi ◽  
M. Konno ◽  
T. Kamino ◽  
M. Ogasawara ◽  
K. Kaji ◽  
...  

Abstract A technique for preparation of a pillar shaped sample and its multi-directional observation of the sample using a focused ion beam (FIB) / scanning transmission electron microscopy (STEM) system has been developed. The system employs an FIB/STEM compatible sample rotation holder with a specially designed rotation mechanism, which allows the sample to be rotated 360 degrees [1-3]. This technique was used for the three dimensional (3D) elemental mapping of a contact plug of a Si device in 90 nm technology. A specimen containing a contact plug was shaped to a pillar sample with a cross section of 200 nm x 200 nm and a 5 um length. Elemental analysis was performed with a 200 kV HD-2300 STEM equipped with the EDAX genesis Energy dispersive X-ray spectroscopy (EDX) system. Spectrum imaging combined with multivariate statistical analysis (MSA) [4, 5] was used to enhance the weak X-ray signals of the doped area, which contain a low concentration of As-K. The distributions of elements, especially the dopant As, were successfully enhanced by MSA. The elemental maps were .. reconstructed from the maps.


1998 ◽  
Vol 4 (S2) ◽  
pp. 856-857
Author(s):  
David M. Longo ◽  
James M. Howe ◽  
William C. Johnson

The focused ion beam (FIB) has become an indispensable tool for a variety of applications in materials science, including that of specimen preparation for the transmission electron microscope (TEM). Several FIB specimen preparation techniques have been developed, but some problems result when FIB specimens are analyzed in the TEM. One of these is X-ray fluorescence from bulk material surrounding the thin membrane in FIB-prepared samples. This paper reports on a new FIB specimen preparation method which was devised for the reduction of X-ray fluorescence during energy dispersive X-ray spectroscopy (EDS) in the TEM.Figure 1 shows three membrane geometries that were investigated in this study on a single-crystal Si substrate with a RF sputter-deposited 50 nm Ni film. Membrane 1 is the most commonly reported geometry in the literature, with an approximately 20 urn wide trench and a membrane having a single wedge with a 1.5° incline.


2000 ◽  
Vol 6 (3) ◽  
pp. 218-223
Author(s):  
Toshie Yaguchi ◽  
Takeo Kamino ◽  
Mitsumasa Sasaki ◽  
Gerard Barbezat ◽  
Ryoichi Urao

Abstract A focused ion beam (FIB) technique was applied to cross-sectional specimen preparation to observe an interface between a plasma sprayed coating and an aluminum (Al) substrate by transmission electron microscopy (TEM). The surface of the sprayed coating film has a roughness of several tens of microns. Sputter rates for the coating film and the substrate are greatly different. The rough surface and the difference in sputter rate cause problems in making TEM specimens with smooth side walls. The top surface of the coating film was planerized by the FIB before fabricating the TEM specimen. The interfaces were investigated by TEM and energy-dispersive X-ray (EDX) analysis. The TEM observation revealed that there is a 10 nm thick amorphous layer at the interface between the coating film and substrate. The coating film consists of two kinds of sublayers with bright and dark contrast. The bright contrast sublayers were amorphous layers with thickness of 2~10 nm. The Al/Fe X-ray intensity ratio was larger in bright contrast sublayers than that in dark contrast sublayers.


1999 ◽  
Vol 5 (S2) ◽  
pp. 908-909
Author(s):  
J.L. Drown-MacDonald ◽  
B.I. Prenitzer ◽  
T.L. Shofner ◽  
L.A. Giannuzzi

Focused Ion Beam (FIB) specimen preparation for both scanning and transmission electron microscopy (SEM and TEM respectively) has seen an increase in usage over the past few years. The advantage to the FIB is that site specific cross sections (or plan view sections) may be fabricated quickly and reproducibly from numerous types of materials using a finely focused beam of Ga+ ions [1,2]. It was demonstrated by Prenitzer et al. that TEM specimens may be acquired from individual Zn powder particles by employing the FIB LO specimen preparation technique [3]. In this paper, we use the FIB LO technique to prepare TEM specimens from Mount Saint Helens volcanic ash.Volcanic ash from Mount Saint Helens was obtained at the Microscopy and Microanalysis 1998 meeting in Atlanta. TEM analysis of the ash was performed using the FIB lift out technique [1]. Ash powders were dusted onto an SEM sample stud that had been coated with silver paint.


Author(s):  
Liang Hong ◽  
Jia Li ◽  
Haifeng Wang

Abstract This paper provides an innovative root cause failure analysis method that combines multiple failure analysis (FA) techniques to narrow down and expose the shorting location and allow the material analysis of the shorting defect. It begins with a basic electrical testing to narrow down shorting metal layers, then utilizing mechanical lapping to expose over coat layers. This is followed by optical beam induced resistance change imaging to further narrow down the shorting location. Scanning electron microscopy and optical imaging are used together with focused ion beam milling to slice and view through the potential shorting area until the shorting defect is exposed. Finally, transmission electron microscopy (TEM) sample is prepared, and TEM analysis is carried out to pin point the root cause of the shorting. This method has been demonstrated successfully on Western Digital inter-metal layers shorting FA.


2010 ◽  
Vol 16 (2) ◽  
pp. 210-217 ◽  
Author(s):  
Xiaoxing Ke ◽  
Sara Bals ◽  
Daire Cott ◽  
Thomas Hantschel ◽  
Hugo Bender ◽  
...  

AbstractThe three-dimensional (3D) distribution of carbon nanotubes (CNTs) grown inside semiconductor contact holes is studied by electron tomography. The use of a specialized tomography holder results in an angular tilt range of ±90°, which means that the so-called “missing wedge” is absent. The transmission electron microscopy (TEM) sample for this purpose consists of a micropillar that is prepared by a dedicated procedure using the focused ion beam (FIB) but keeping the CNTs intact. The 3D results are combined with energy dispersive X-ray spectroscopy (EDS) to study the relation between the CNTs and the catalyst particles used during their growth. The reconstruction, based on the full range of tilt angles, is compared with a reconstruction where a missing wedge is present. This clearly illustates that the missing wedge will lead to an unreliable interpretation and will limit quantitative studies.


1999 ◽  
Vol 5 (5) ◽  
pp. 365-370 ◽  
Author(s):  
Toshie Yaguchi ◽  
Takeo Kamino ◽  
Tohru Ishitani ◽  
Ryoichi Urao

A new method for transmission electron microscope (TEM) specimen preparation using a focused ion beam (FIB) system that results in a lower rate of gallium (Ga) implantation has been developed. The method was applied to structural and analytical studies of composite materials such as silicon (Si)-devices and magneto-optical disk. To protect the specimens against Ga ion irradiation, amorphous tungsten (W) was deposited on the surface of the specimen prior to FIB milling. The deposition was quite effective in reducing the Ga implantation rate, and energy-dispersive X-ray (EDX) analysis of these specimens detected 0.3Ð1.5% Ga incorporated in the thinned area. FIB milling times for these specimens were 1.5Ð2 hr. Although the milling rate was high, all the materials were properly prepared for TEM study, and clear crystal lattice images were observed on all specimens.


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