Microstructural Characterization of Automated Specimen Preparation for TEM Analysis

2000 ◽  
Vol 6 (S2) ◽  
pp. 528-529
Author(s):  
C. Urbanik Shannon ◽  
L. A. Giannuzzi ◽  
E. M. Raz
Keyword(s):  
Focused Ion Beam ◽  
Preparation Method ◽  
Ion Beam ◽  
Microstructural Characterization ◽  
Specimen Preparation ◽  
Tem Analysis ◽  
Area Of Interest ◽  
Transmission Electron ◽  
Preparation Techniques

Automated specimen preparation for transmission electron microscopy has the obvious advantage of saving personnel time. While some people may perform labor intensive specimen preparation techniques quickly, automated specimen preparation performed in a timely and reproducible fashion can significantly improve the throughput of specimens in an industrial laboratory. The advent of focused ion beam workstations for the preparation of electron transparent membranes has revolutionized TEM specimen preparation. The FIB lift-out technique is a powerful specimen preparation method. However, there are instances where the “traditional” FIB method of specimen preparation may be more suitable. The traditional FIB method requires that specimens must be prepared so that the area of interest is as thin as possible (preferably less than 50 μm) prior to FIB milling. Automating the initial specimen preparation for brittle materials (e.g., Si wafers) may be performed using the combination of cleaving and sawing techniques as described below.

Characterization of FIB Damage in Silicon

1999 ◽  
Vol 5 (S2) ◽  
pp. 740-741 ◽  
Author(s):  
C.A. Urbanik ◽  
B.I. Prenitzer ◽  
L.A. Gianhuzzi ◽  
S.R. Brown ◽  
T.L. Shofner ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Target Material ◽  
Beam Current ◽  
Specimen Preparation ◽  
Transfer Energy ◽  
Transmission Electron ◽  
Preparation Techniques ◽  
Reactive Gas

Focused ion beam (FIB) instruments are useful for high spatial resolution milling, deposition, and imaging capabilities. As a result, FIB specimen preparation techniques have been widely accepted within the semiconductor community as a means to rapidly prepare high quality, site-specific specimens for transmission electron microscopy (TEM) [1]. In spite of the excellent results that have been observed for both high resolution (HREM) and standard TEM specimen preparation applications, a degree of structural modification is inherent to FIB milled surfaces [2,3]. The magnitude of the damage region that results from Ga+ ion bombardment is dependent on the operating parameters of the FIB (e.g., beam current, beam voltage, milling time, and the use of reactive gas assisted etching).Lattice defects occur as a consequence of FIB milling because the incident ions transfer energy to the atoms of the target material. Momentum transferred from the incident ions to the target atoms can result in the creation of point defects (e.g., vacancies, self interstitials, and interstitial and substitutional ion implantation), the generation of phonons, and plasmon excitation in the case of metal targets.

scholarly journals Using a Focused Ion Beam (FIB) System to Extract TEM-Ready Samples from Complex Metallic and Ceramic Structures

1999 ◽  
Vol 7 (2) ◽  
pp. 12-15 ◽  
Author(s):  
Lucille A. Giannuzzi ◽  
Richard Young ◽  
Pete Carleson
Keyword(s):  
Focused Ion Beam ◽  
Preparation Method ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Magnetic Media ◽  
Tem Analysis ◽  
Micro Fabrication ◽  
Site Specific ◽  
Transmission Electron ◽  
Two Sides

AbstractDriven by the analytical needs of microelectronics, magnetic media and micro-fabrication industries, focused ion beam (FIB) systems are now capable of milling and manipulating samples for the analysis of microstructure features having dimensions of 180 nm or less, A technique for locating and extracting site specific specimens for examination by transmission electron microscopy (TEM) has been developed. An identified feature can be located and precisely milled with an FIB system from two sides to prepare an ultrathin sample, and then extracted from the region with a glass rod micromanipulator onto a grid for TEM analysis. This specimen preparation method has been applied to semiconductor failure analysis and to the study of metallic and ceramic microsiructures with irregular topographies and complex mufti-layered components.

TEM Specimen Preparation of Oxidized Ni-Base Alloys using the Focused Ion Beam (FIB) Technique

2000 ◽  
Vol 6 (S2) ◽  
pp. 540-541
Author(s):  
K.L. More ◽  
D.W. Coffey ◽  
B.A. Pint ◽  
K.S. Trent ◽  
P.F. Tortorelli
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Microstructural Characterization ◽  
Alumina Scale ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Transmission Electron ◽  
The Many ◽  
Native Surface

Microstructural characterization of thin alumina scales formed on oxidized Ni-base alloys using transmission electron microscopy (TEM) has long been a challenge as a result of the many problems encountered during the preparation of thin specimens. Successful and reproducible preparation of uniformly thin, cross-section TEM specimens from these multicomponent “layered” structures (alumina scale on a metallic substrate) is extremely difficult using standard ion beam thinning procedures for several reasons: (1) differential thinning of the various constituents in the system can occur, (2) a weak ceramic-metal interface may lead to separation during the harsh mechanical grinding and thinning procedure, (3) fully intact scales are rarely achieved since native surface structures are usually lost during ion milling, and (4) extensive damage can be created in the scale and alloy during rough grinding and polishing steps as well as during final ion beam thinning.

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.

Comparison of Precision XTEM Specimen Preparation Techniques for Semiconductor Failure Analysis

1997 ◽  
Vol 3 (S2) ◽  
pp. 357-358
Author(s):  
C. Amy Hunt
Keyword(s):  
Sample Preparation ◽  
Failure Analysis ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Mechanical Polishing ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Tem Analysis ◽  
The Past ◽  
Preparation Techniques

The demand for TEM analysis in semiconductor failure analysis is rising sharply due to the shrinking size of devices. A well-prepared sample is a necessity for getting meaningful results. In the past decades, a significant amount of effort has been invested in improving sample preparation techniques for TEM specimens, especially precision cross-sectioning techniques. The most common methods of preparation are mechanical dimpling & ion milling, focused ion beam milling (FIBXTEM), and wedge mechanical polishing. Each precision XTEM technique has important advantages and limitations that must be considered for each sample.The concept for both dimpling & ion milling and wedge specimen preparation techniques is similar. Both techniques utilize mechanical polishing to remove the majority of the unwanted material, followed by ion milling to assist in final polishing or cleaning. Dimpling & ion milling produces the highest quality samples and is a relatively easy technique to master.

Focused Ion Beam Milling and Micromanipulation Lift-Out for Site Specific Cross-Section Tem Specimen Preparation

1997 ◽  
Vol 480 ◽  
Author(s):  
L. A. Giannuzzi ◽  
J. L. Drown ◽  
S. R. Brown ◽  
R. B. Irwin ◽  
F. A. Stevie
Keyword(s):  
Cross Section ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specific Area ◽  
Specimen Preparation ◽  
Tem Analysis ◽  
Site Specific ◽  
Area Of Interest ◽  
Carbon Coated ◽  
A Site

AbstractA site specific technique for cross-section transmission electron microscopy specimen preparation of difficult materials is presented. Focused ion beams are used to slice an electron transparent sliver of the specimen from a specific area of interest. Micromanipulation lift-out procedures are then used to transport the electron transparent specimen to a carbon coated copper grid for subsequent TEM analysis. The experimental procedures are described in detail and an example of the lift-out technique is presented.

TEM FIB Lift-Out of Mount Saint Helens Volcanic Ash

1999 ◽  
Vol 5 (S2) ◽  
pp. 908-909
Author(s):  
J.L. Drown-MacDonald ◽  
B.I. Prenitzer ◽  
T.L. Shofner ◽  
L.A. Giannuzzi
Keyword(s):  
Cross Sections ◽  
Volcanic Ash ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Preparation Technique ◽  
Tem Analysis ◽  
Plan View ◽  
Transmission Electron ◽  
Silver Paint

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.

scholarly journals Combined Focused Ion Beam-Ultramicrotomy Method for TEM Specimen Preparation of Porous Fine-Grained Materials

2019 ◽  
Vol 26 (1) ◽  
pp. 120-125 ◽  
Author(s):  
Kenta K. Ohtaki ◽  
Hope A. Ishii ◽  
John P. Bradley
Keyword(s):  
Focused Ion Beam ◽  
Preparation Method ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Combined Method ◽  
Fine Grained ◽  
Heterogeneous Samples ◽  
Transmission Electron ◽  
Fine Grained Material ◽  
The One

AbstractA new transmission electron microscopy (TEM) specimen preparation method that utilizes a combination of focused ion beam (FIB) methods and ultramicrotomy is demonstrated. This combined method retains the benefit of site-specific sampling by FIB but eliminates ion beam-induced damage except at specimen edges and allows recovery of many consecutive sections. It is best applied to porous and/or fine-grained materials that are amenable to ultramicrotomy but are located in bulk samples that are not. The method is ideal for unique samples from which every specimen is precious, and we demonstrate its utility on fine-grained material from the one-of-a-kind Paris meteorite. Compared with a specimen prepared by conventional FIB methods, the final sections are uniformly thin and free from re-deposition and curtaining artifacts common in FIB specimens prepared from porous, heterogeneous samples.

Microstructural Characterization of Dehydrogenated Products of the LiBH4-YH3 Composite

2014 ◽  
Vol 20 (6) ◽  
pp. 1798-1804 ◽  
Author(s):  
Ji Woo Kim ◽  
Kee-Bum Kim ◽  
Jae-Hyeok Shim ◽  
Young Whan Cho ◽  
Kyu Hwan Oh
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Microstructural Characterization ◽  
Static Vacuum ◽  
Lithium Borohydride ◽  
Transmission Electron ◽  
Resolution Imaging ◽  
Yttrium Hydride ◽  
Beam Technique

AbstractThe dehydrogenated microstructure of the lithium borohydride-yttrium hydride (LiBH4-YH3) composite obtained at 350°C under 0.3 MPa of hydrogen and static vacuum was investigated by transmission electron microscopy combined with a focused ion beam technique. The dehydrogenation reaction between LiBH4 and YH3 into LiH and YB4 takes place under 0.3 MPa of hydrogen, which produces YB4 nano-crystallites that are uniformly distributed in the LiH matrix. This microstructural feature seems to be beneficial for rehydrogenation of the dehydrogenation products. On the other hand, the dehydrogenation process is incomplete under static vacuum, leading to the unreacted microstructure, where YH3 and YH2 crystallites are embedded in LiBH4 matrix. High resolution imaging confirmed the presence of crystalline B resulting from the self-decomposition of LiBH4. However, Li2B12H12, which is assumed to be present in the LiBH4 matrix, was not clearly observed.

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