Comparison of Focused Ion Beam and Conventional Techniques on Tem Specimen Preparation of Metal-Ceramic Interfaces

1998 ◽  
Vol 4 (S2) ◽  
pp. 860-861 ◽  
Author(s):  
A. Ramirez de Arellano López ◽  
W.-A. Chiou ◽  
K. T. Faber
Keyword(s):  
Focused Ion Beam ◽  
Ceramic Coating ◽  
Steel Substrate ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Inhomogeneous Materials ◽  
Cross Sectional ◽  
Fine Grain ◽  
Basic Industry ◽  
Coated Surface

The results of TEM analyses of materials are critically dependent on the quality of the sample prepared. Although numerous techniques have been developed in the last two decades, differential thinning of inhomogeneous materials remains a serious problem. Recently, focused ion beam (FIB) technique has been introduced for cross-sectional sample preparation for TEM and SEM.A novel system for depositing a fine-grain (∼ 200 nm) ceramic coating on a metal surface via a patent pending Small-Particle Plasma Spray (SPPS) technique has been developed at the Basic Industry Research Laboratory of Northwestern University. To understand the properties of the coated surface, the ceramic/metal interface and the microstructure of the ceramic coating must be investigated. This paper presents a comparison of the microstructure of an A12O3 coating on a mild steel substrate prepared using conventional and FEB techniques.

Method for Cross-sectional Thin Specimen Preparation from a Specific Site Using a Combination of a Focused Ion Beam System and Intermediate Voltage Electron Microscope and Its Application to the Characterization of a Precipitate in a Steel

2001 ◽  
Vol 7 (3) ◽  
pp. 287-291
Author(s):  
Toshie Yaguchi ◽  
Hiroaki Matsumoto ◽  
Takeo Kamino ◽  
Tohru Ishitani ◽  
Ryoichi Urao
Keyword(s):  
Electron Microscope ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specific Site ◽  
Specimen Preparation ◽  
Thin Specimen ◽  
Cross Sectional ◽  
Electron Detector ◽  
Specimen Holder

AbstractIn this study, we discuss a method for cross-sectional thin specimen preparation from a specific site using a combination of a focused ion beam (FIB) system and an intermediate voltage transmission electron microscope (TEM). A FIB-TEM compatible specimen holder was newly developed for the method. The thinning of the specimen using the FIB system and the observation of inside structure of the ion milled area in a TEM to localize a specific site were alternately carried out. The TEM fitted with both scanning transmitted electron detector and secondary electron detector enabled us to localize the specific site in a halfway milled specimen with the positional accuracy of better than 0.1 µm. The method was applied to the characterization of a precipitate in a steel. A submicron large precipitate was thinned exactly at its center for the characterization by a high-resolution electron microscopy and an elemental mapping.

A Method for Site Specific Characterization Using a Dedicated FIB System Combined With an Analyitical TEM

1999 ◽  
Vol 5 (S2) ◽  
pp. 914-915
Author(s):  
T. Kamino ◽  
T. Yaguchi ◽  
H. Matsumoto ◽  
H. Kobayashi ◽  
H. Koike
Keyword(s):  
Focused Ion Beam ◽  
Ion Irradiation ◽  
Ion Beam ◽  
System Stability ◽  
Specimen Preparation ◽  
Thin Specimen ◽  
Cross Sectional ◽  
Site Specific ◽  
Specimen Holder ◽  
High Resolution Tem

A method for site specific characterization of the materials using a dedicated focused ion beam(FIB) system and an analytical transmission electron microscope (TEM) was developed. Needless to say, in TEM specimen preparation using FIB system, stability of a specimen is quite important. The specimen stage employed in the developed FIB system is the one designed for high resolution TEM, and the specimen drift rate of the stage is less than lnm/min. In addition, FIB-TEM compatible specimen holder which allows milling of a specimen with the FIB system and observation of the specimen with the TEM without re-loading was developed. To obtain thin specimen from the area to be characterized correctly, confirmation of the area before final milling is needed. However, observation of cross sectional view in a FIB system is recommended because it causes damage by Ga ion irradiation. To solve this problem, we used a STEM unit as a viewer of FIB milled specimen.

Cross-sectional Specimen Preparation and Observation of a Plasma Sprayed Coating Using a Focused Ion Beam/Transmission Electron Microscopy System

2000 ◽  
Vol 6 (3) ◽  
pp. 218-223
Author(s):  
Toshie Yaguchi ◽  
Takeo Kamino ◽  
Mitsumasa Sasaki ◽  
Gerard Barbezat ◽  
Ryoichi Urao
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Coating Film ◽  
Cross Sectional ◽  
X Ray ◽  
Bright Contrast ◽  
Transmission Electron ◽  
Sprayed Coating ◽  
Plasma Sprayed

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.

Cross-Sectional TEM Specimen Preparation of Semiconductor Devices by Focused Ion Beam Etching

1990 ◽  
Vol 199 ◽  
Author(s):  
Kyung-ho Park
Keyword(s):  
Integrated Circuit ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Semiconductor Devices ◽  
Standard Technique ◽  
Specimen Preparation ◽  
Cross Sectional ◽  
Ion Beam Etching ◽  
Submicron Scale ◽  
A New Technique

ABSTRACTA procedure for preparing cross-sectional TEM specimens by focused ion beam etching (FIB) of specific regions on an integrated circuit chip is outlined. The investigation of the morphology, structure and local chemistry of precisely selected regions of semiconductor devices becomes increasingly important since the lateral dimensions and layer thickness of device structures are continually being reduced. The standard technique of preparing specimens for TEM, whether planar or cross-sectional, cannot select particular small regions. Some techniques and a number of tools and fixtures have been proposed which allow us to prepare TEM specimen of prespecified locations in complex devices. Most of these techniques, however, are still very difficult, tedious process and time consuming.A new technique has been proposed recently involving the use of FIB. The technique ensures that the preselected area of submicron scale will be located in the electron transparent section used for TEM imaging, in preparation turn-around time of about two hours. The TEM imaging of specific contacts via hole in a VLSI chip is illustrated.

Method for Cross-sectional Transmission Electron Microscopy Specimen Preparation of Composite Materials Using a Dedicated Focused Ion Beam System

1999 ◽  
Vol 5 (5) ◽  
pp. 365-370 ◽  
Author(s):  
Toshie Yaguchi ◽  
Takeo Kamino ◽  
Tohru Ishitani ◽  
Ryoichi Urao
Keyword(s):  
Composite Materials ◽  
Focused Ion Beam ◽  
Ion Irradiation ◽  
Ion Beam ◽  
Implantation Rate ◽  
Specimen Preparation ◽  
Cross Sectional ◽  
X Ray ◽  
Transmission Electron ◽  
Lattice Images

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.

Cross-sectional Specimen Preparation and Observation of a Plasma Sprayed Coating Using a Focused Ion Beam/Transmission Electron Microscopy System

2000 ◽  
Vol 6 (3) ◽  
pp. 218-223 ◽  
Author(s):  
Toshie Yaguchi ◽  
Takeo Kamino ◽  
Mitsumasa Sasaki ◽  
Gerard Barbezat ◽  
Ryoichi Urao
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Coating Film ◽  
Cross Sectional ◽  
X Ray ◽  
Bright Contrast ◽  
Transmission Electron ◽  
Sprayed Coating ◽  
Plasma Sprayed

AbstractA 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.

Application of Focused Ion Beam to Atom Probe Tomography Specimen Preparation from Mechanically Alloyed Powders

2007 ◽  
Vol 13 (5) ◽  
pp. 347-353 ◽  
Author(s):  
Pyuck-Pa Choi ◽  
Tala'at Al-Kassab ◽  
Young-Soon Kwon ◽  
Ji-Soon Kim ◽  
Reiner Kirchheim
Keyword(s):  
Atom Probe Tomography ◽  
Structural Changes ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Atom Probe ◽  
High Energy ◽  
Specimen Preparation ◽  
Mechanically Alloyed ◽  
Cross Sectional ◽  
Beam Currents

Focused ion-beam milling has been applied to prepare needle-shaped atom probe tomography specimens from mechanically alloyed powders without the use of embedding media. The lift-out technique known from transmission electron microscopy specimen preparation was modified to cut micron-sized square cross-sectional blanks out of single powder particles. A sequence of rectangular cuts and annular milling showed the highest efficiency for sharpening the blanks to tips. First atom probe results on a Fe95Cu5 powder mechanically alloyed in a high-energy planetary ball mill for 20 h have been obtained. Concentration profiles taken from this powder sample showed that the Cu distribution is inhomogeneous on a nanoscale and that the mechanical alloying process has not been completed yet. In addition, small clusters of oxygen, stemming from the ball milling process, have been detected. Annular milling with 30 keV Ga ions and beam currents ≥50 pA was found to cause the formation of an amorphous surface layer, whereas no structural changes could be observed for beam currents ≤10 pA.

Contact damage evolution in diamondlike carbon coatings on ductile substrates

2008 ◽  
Vol 23 (1) ◽  
pp. 27-36 ◽  
Author(s):  
Rajnish K. Singh ◽  
M.T. Tilbrook ◽  
Z.H. Xie ◽  
A. Bendavid ◽  
P.J. Martin ◽  
...  
Keyword(s):  
Damage Evolution ◽  
Focused Ion Beam ◽  
Steel Substrate ◽  
Ion Beam ◽  
Chemical Vapor ◽  
Displacement Curve ◽  
Coating System ◽  
Cross Sectional ◽  
Diamondlike Carbon ◽  
Load Displacement

A diamondlike carbon (DLC) thin film was deposited onto a stainless steel substrate using a plasma-enhanced chemical vapor deposition (PECVD) process. Nanoindentation, coupled with focused-ion-beam (FIB) milling, was used to investigate contact-induced deformation and fracture in this coating system. Following initial elastic contact between the coating and the indenter and apparent plastic yield of the substrate, pop-ins were observed in the load–displacement curve, indicative of coating fracture. However, FIB cross-sectional images of indentations revealed the presence of ring, radial, and lateral cracks at loads much lower than the critical load for the first observed pop-ins. Finite element modeling was used, and the properties of the substrate and the film were calibrated by fitting the simulated load–displacement curves to experimental data. Then, based upon the experimental observations of damage evolution in this coating system, the stress distributions relevant to initiate ring, radial, and lateral cracks in the coating were ascertained. Furthermore, the effects of substrate yield stress and coating residual stress on the formation of these cracks were investigated.

A Preparation Method of Diamond Specimens Using an Advanced FIB Microscopy for Micro and Nanoanalysis

2012 ◽  
Vol 531-532 ◽  
pp. 592-595
Author(s):  
Yi Qing Chen ◽  
Feng Zai Tang ◽  
Liang Chi Zhang
Keyword(s):  
Focused Ion Beam ◽  
Preparation Method ◽  
Ion Beam ◽  
Polycrystalline Diamond ◽  
Specimen Preparation ◽  
Atomic Lattice ◽  
Cross Sectional ◽  
Site Specific ◽  
Dual Beam

This paper reports the specimen preparation using an advanced dual beam focused ion beam (FIB) technique for bulk polycrystalline diamond (PCD) composites after dynamic friction polishing (DFP). The technique adapted allows for precisely processing diamond materials at the specific polishing track sites of PCD surface, from which large cross-sectional specimens for SEM/EDS/Raman microanalysis could be successfully created. In addition, an in-situ lift-out method was developed to prepare the site-specific HRTEM specimens which were thin enough for imaging the atomic lattice of diamond and for conducting EELS analysis.

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