Three-Dimensional Analysis of Carbon Nanotube Networks in Interconnects by Electron Tomography without Missing Wedge Artifacts

2010 ◽  
Vol 16 (2) ◽  
pp. 210-217 ◽  
Author(s):  
Xiaoxing Ke ◽  
Sara Bals ◽  
Daire Cott ◽  
Thomas Hantschel ◽  
Hugo Bender ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Electron Tomography ◽  
Ion Beam ◽  
Full Range ◽  
Three Dimensional ◽  
X Ray ◽  
Quantitative Studies ◽  
Transmission Electron ◽  
Carbon Nanotube Networks ◽  
Semiconductor Contact

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.

3D Observation of Elemental Distribution of Si-Device using a Dedicated FIB/STEM System

2005 ◽  
Author(s):  
T. Yaguchi ◽  
M. Konno ◽  
T. Kamino ◽  
M. Ogasawara ◽  
K. Kaji ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Three Dimensional ◽  
Elemental Distribution ◽  
Multivariate Statistical ◽  
X Ray ◽  
Sample Rotation ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Elemental Maps

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.

scholarly journals Automated cryo-lamella preparation for high-throughput in-situ structural biology

2019 ◽  
Author(s):  
Genevieve Buckley ◽  
Gediminas Gervinskas ◽  
Cyntia Taveneau ◽  
Hari Venugopal ◽  
James C. Whisstock ◽  
...  
Keyword(s):  
Saccharomyces Cerevisiae ◽  
Structural Biology ◽  
Focused Ion Beam ◽  
Electron Tomography ◽  
Ion Beam ◽  
Automated Method ◽  
Cellular Environment ◽  
Transmission Electron

AbstractCryo-transmission electron tomography (cryo-ET) in association with cryo-focused ion beam (cryo-FIB) milling enables structural biology studies to be performed directly within the cellular environment. Cryo-preserved cells are milled and a lamella with a thickness of 200-300 nm provides an electron transparent window suitable for cryo-ET imaging. Cryo-FIB milling is an effective method, but it is a tedious and time-consuming process, which typically results in ~10 lamellae per day. Here, we introduce an automated method to reproducibly prepare cryo-lamellae on a grid and reduce the amount of human supervision. We tested the routine on cryo-preserved Saccharomyces cerevisiae and demonstrate that this method allows an increased throughput, achieving a rate of 5 lamellae/hour without the need to supervise the FIB milling. We demonstrate that the quality of the lamellae is consistent throughout the preparation and their compatibility with cryo-ET analyses.

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
Keyword(s):  
Intermetallic Compound ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Liquid Aluminium ◽  
Thin Specimen ◽  
Tem Analysis ◽  
X Ray ◽  
Cell Parameters ◽  
Transmission Electron ◽  
Aluminized Steel

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.

The Effect of Focused Ion Beam (Fib) Specimen Geometry on X-Ray Fluorescence During Energy Dispersive X-Ray Spectroscopy (EDS) Analysis in the Transmission Electron Microscope (TEM)

1998 ◽  
Vol 4 (S2) ◽  
pp. 856-857
Author(s):  
David M. Longo ◽  
James M. Howe ◽  
William C. Johnson
Keyword(s):  
Electron Microscope ◽  
Transmission Electron Microscope ◽  
Focused Ion Beam ◽  
Materials Science ◽  
Bulk Material ◽  
Ion Beam ◽  
Energy Dispersive ◽  
Specimen Preparation ◽  
X Ray ◽  
Transmission Electron

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.

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.

Intergrowth of Components and Ramps in Coffin-Shaped ZSM-5 Zeolite Crystals Unraveled by Focused Ion Beam-Assisted Transmission Electron Microscopy

2013 ◽  
Vol 20 (1) ◽  
pp. 42-49 ◽  
Author(s):  
Jiangbo Lu ◽  
Maarten B.J. Roeffaers ◽  
Evelyne Bartholomeeusen ◽  
Bert F. Sels ◽  
Dominique Schryvers
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Main Part ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Three Dimensional ◽  
Orientation Relationships ◽  
Displacement Boundary ◽  
Transmission Electron ◽  
Rotational Components

AbstractScanning electron microscopy, focused ion beam (FIB), and transmission electron microscopy are combined to study the intergrowth of 90° rotational components and of ramps in coffin-shaped ZSM-5 crystals. The 90° rotational boundaries with local zig-zag features between different intergrowth components are observed in the main part of crystal. Also a new kind of displacement boundary is described. At the displacement boundary there is a shift of the unit cells along the boundary without a change in orientation. Based on lamellae prepared with FIB from different positions of the ramps and crystal, the orientation relationships between ramps and the main part of the crystal are studied and the three-dimensional morphology and growth mechanism of the ramp are illustrated.

scholarly journals Stem-EDX and FIB-SEM Tomography of ALLVAC 718Plus Superalloy

2016 ◽  
Vol 61 (2) ◽  
pp. 535-542 ◽  
Author(s):  
A. Kruk ◽  
G. Cempura ◽  
S. Lech ◽  
A. Czyrska -Filemonowicz
Keyword(s):  
Electron Microscope ◽  
Focused Ion Beam ◽  
Electron Tomography ◽  
Ion Beam ◽  
High Strength ◽  
Strengthening Mechanism ◽  
Scanning Transmission Electron Microscope ◽  
Particle Analysis ◽  
Transmission Electron ◽  
Scanning Transmission

Abstract Allvac 718Plus (718Plus) is a high strength, corrosion resistant nickel- based superalloy used for application in power generation, aeronautics and aerospace industry. The 718Plus microstructure consists of a γ matrix with γ’-Ni3(Al,Ti) and some δ- Ni3Nb phases as well as lamellar particles (η-Ni3Ti, η*-Ni6AlNb or Ni6(Al,Ti)Nb) precipitated at the grain boundaries. The primary strengthening mechanism for this alloy is a precipitation hardening, therefore size and distribution of precipitates are critical for the performance of the alloy. The aim of this study was to characterize precipitates in the 718Plus superalloy using Scanning Transmission Electron Microscope combined with Energy Dispersive X-ray Spectroscopy (STEM-EDX) and Focused Ion Beam Scanning Electron Microscope (FIB-SEM). The STEM-EDX and FIB-SEM tomography techniques were used for 3D imaging and metrology of the precipitates. Transmission electron microscopy and EDX spectroscopy were used to reveal details of the 718Plus microstructure and allow determine chemical composition of the phases. The study showed that electron tomography techniques permit to obtain complementary information about microstructural features (precipitates size, shape and their 3D distribution) in the reconstructed volume with comparison to conventional particle analysis methods, e.g. quantitative TEM and SEM metallography

scholarly journals From tissue retrieval to electron tomography: nanoscale characterization of the interface between bone and bioactive glass

2021 ◽  
Vol 18 (182) ◽  
pp. 20210181
Author(s):  
Chiara Micheletti ◽  
Pedro Henrique Silva Gomes-Ferreira ◽  
Travis Casagrande ◽  
Paulo Noronha Lisboa-Filho ◽  
Roberta Okamoto ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Bioactive Glass ◽  
Focused Ion Beam ◽  
Electron Tomography ◽  
Ion Beam ◽  
Three Dimensions ◽  
Transmission Electron Microscopy Analysis ◽  
Dental Procedures ◽  
Transmission Electron

The success of biomaterials for bone regeneration relies on many factors, among which osseointegration plays a key role. Biogran (BG) is a bioactive glass commonly employed as a bone graft in dental procedures. Despite its use in clinical practice, the capability of BG to promote osseointegration has never been resolved at the nanoscale. In this paper, we present the workflow for characterizing the interface between newly formed bone and BG in a preclinical rat model. Areas of bone–BG contact were first identified by backscattered electron imaging in a scanning electron microscope. A focused ion beam in situ lift-out protocol was employed to prepare ultrathin samples for transmission electron microscopy analysis. The bone–BG gradual interface, i.e. the biointerphase, was visualized at the nanoscale with unprecedented resolution thanks to scanning transmission electron microscopy. Finally, we present a method to view the bone–BG interface in three dimensions using electron tomography.

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