scholarly journals Method of Ga removal from a specimen on a microelectromechanical system-based chip for in-situ transmission electron microscopy

2020 ◽  
Vol 50 (1) ◽  
Author(s):  
Yena Kwon ◽  
Byeong-Seon An ◽  
Yeon-Ju Shin ◽  
Cheol-Woong Yang
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ion Beam ◽  
Thin Foil ◽  
Ex Situ ◽  
Ion Milling ◽  
Microelectromechanical System ◽  
Transmission Electron ◽  
Foil Specimen

Abstract In-situ transmission electron microscopy (TEM) holders that employ a chip-type specimen stage have been widely utilized in recent years. The specimen on the microelectromechanical system (MEMS)-based chip is commonly prepared by focused ion beam (FIB) milling and ex-situ lift-out (EXLO). However, the FIB-milled thin-foil specimens are inevitably contaminated with Ga+ ions. When these specimens are heated for real time observation, the Ga+ ions influence the reaction or aggregate in the protection layer. An effective method of removing the Ga residue by Ar+ ion milling within FIB system was explored in this study. However, the Ga residue remained in the thin-foil specimen that was extracted by EXLO from the trench after the conduct of Ar+ ion milling. To address this drawback, the thin-foil specimen was attached to an FIB lift-out grid, subjected to Ar+ ion milling, and subsequently transferred to an MEMS-based chip by EXLO. The removal of the Ga residue was confirmed by energy dispersive spectroscopy.

scholarly journals A method of Ga removal from a specimen fabricated on MEMS-based chip for in-situ transmission electron microscopy

2020 ◽  
Author(s):  
Yena Kwon ◽  
Byeong-Seon An ◽  
Yeon-Ju Shin ◽  
Cheol-Woong Yang
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ion Beam ◽  
Thin Foil ◽  
Type Specimen ◽  
Ex Situ ◽  
Ion Milling ◽  
Transmission Electron ◽  
Foil Specimen

Abstract In-situ transmission electron microscopy (TEM) holders, which are widely used in recent years, employ a chip-type specimen stage. To prepare the specimen on the microelectromechanical system (MEMS)-based chip, focused ion beam (FIB) and ex-situ lift-out (EXLO) techniques has been widely used. However, thin foil specimens prepared using the FIB inevitably contain the contamination induced by Ga+ ions. In particular, when the specimen is heated for real time observation, it is observed that Ga+ ions influence the reaction or aggregate in the protection layer. An effective method of removing the Ga residue is demonstrated using Ar+ ion milling within FIB. In the case of lifting the thin foil specimen from the trench by the EXLO technique, Ga still remained even if Ar+ ion milling was conducted. To avoid this problem, the thin foil specimen was attached to FIB lift-out grid, performing Ar+ ion milling, and then transferred to a MEMS chip using EXLO technique. The removal of the Ga residue was confirmed using energy dispersive spectroscopy (EDS).

In-Situ Transmission Electron Microscopy of the Solid-Phase Epitaxial Growth of GaAs: Sample Preparation and Artifact Characterization

1997 ◽  
Vol 480 ◽  
Author(s):  
K. B. Belay ◽  
M. C. Ridgway ◽  
D. J. Llewellyn
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Epitaxial Growth ◽  
Solid Phase ◽  
Ion Beam ◽  
Ex Situ ◽  
In Situ Tem ◽  
Transmission Electron

AbstractIn-situ transmission electron microscopy (TEM) has been used to characterize the solidphase epitaxial growth of amorphized GaAs at a temperature of 260°C. To maximize heat transfer from the heated holder to the sample and minimize electron-irradiation induced artifacts, non-conventional methodologies were utilized for the preparation of cross-sectional samples. GaAs (3xI) mm rectangular slabs were cut then glued face-to-face to a size of (6x3) mm stack by maintaining the TEM region at the center. This stack was subsequently polished to a thickness of ~ 200 ýtm. A 3 mm disc was then cut from it using a Gatan ultrasonic cutter. The disc was polished and dimpled on both sides to a thickness of ~15 mimT.h is was ion-beam milled at liquid nitrogen temperature to an electron-transparent layer. From a comparison of in-situ and ex-situ measurements of the recrystallization rate, the actual sample temperature during in-situ characterization was estimated to deviate by ≤ 20°C from that of the heated holder. The influence of electron-irradiated was found to be negligible by comparing the recrystallization rate and microstructure of irradiated and unirradiated regions of comparable thickness. Similarly, the influence of “thin-foil effect” was found to be negligible by comparing the recrystallization rate and microstructure of thick and thin regions, the former determined after the removal of the sample from the microscope and further ion-beam milling of tens of microns of material. In conclusion, the potential influence of artifacts during in-situ TEM can be eliminated by the appropriate choice of sample preparation procedures.

Transmission Electron Microscopy of Epitaxial silicides grown by ultra high vacuum deposition

1989 ◽  
Vol 47 ◽  
pp. 462-463
Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Electron Diffraction ◽  
High Vacuum ◽  
High Energy ◽  
Energy Electron ◽  
Ultra High Vacuum ◽  
Ex Situ ◽  
Transmission Electron

The silicides CoSi2 and NiSi2 are both metallic with the fee flourite structure and lattice constants which are close to silicon (1.2% and 0.6% smaller at room temperature respectively) Consequently epitaxial cobalt and nickel disilicide can be grown on silicon. If these layers are formed by ultra high vacuum (UHV) deposition (also known as molecular beam epitaxy or MBE) their thickness can be controlled to within a few monolayers. Such ultrathin metal/silicon systems have many potential applications: for example electronic devices based on ballistic transport. They also provide a model system to study the properties of heterointerfaces. In this work we will discuss results obtained using in situ and ex situ transmission electron microscopy (TEM).In situ TEM is suited to the study of MBE growth for several reasons. It offers high spatial resolution and the ability to penetrate many monolayers of material. This is in contrast to the techniques which are usually employed for in situ measurements in MBE, for example low energy electron diffraction (LEED) and reflection high energy electron diffraction (RHEED), which are both sensitive to only a few monolayers at the surface.

scholarly journals Direct Characterization of the Relation between the Mechanical Response and Microstructure Evolution in Aluminum by Transmission Electron Microscopy In Situ Straining

Materials ◽  
2021 ◽  
Vol 14 (6) ◽  
pp. 1431
Author(s):  
Seiichiro Ii ◽  
Takero Enami ◽  
Takahito Ohmura ◽  
Sadahiro Tsurekawa
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ion Beam ◽  
Elastic Behavior ◽  
Annealed Specimen ◽  
Displacement Curve ◽  
Dislocation Loops ◽  
Transmission Electron ◽  
Stress Drops

Transmission electron microscopy in situ straining experiments of Al single crystals with different initial lattice defect densities have been performed. The as-focused ion beam (FIB)-processed pillar sample contained a high density of prismatic dislocation loops with the <111> Burgers vector, while the post-annealed specimen had an almost defect-free microstructure. In both specimens, plastic deformation occurred with repetitive stress drops (∆σ). The stress drops were accompanied by certain dislocation motions, suggesting the dislocation avalanche phenomenon. ∆σ for the as-FIB Al pillar sample was smaller than that for the post-annealed Al sample. This can be considered to be because of the interaction of gliding dislocations with immobile prismatic dislocation loops introduced by the FIB. The reloading process after stress reduction was dominated by elastic behavior because the slope of the load–displacement curve for reloading was close to the Young’s modulus of Al. Microplasticity was observed during the load-recovery process, suggesting that microyielding and a dislocation avalanche repeatedly occurred, leading to intermittent plasticity as an elementary step of macroplastic deformation.

Transmission Electron Microscopy of Semiconductor Based Products

1998 ◽  
Vol 523 ◽  
Author(s):  
John Mardinly ◽  
David W. Susnitzky
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ion Beam ◽  
Semiconductor Industry ◽  
Size Reduction ◽  
Specimen Preparation ◽  
Specimen Thickness ◽  
Ion Milling ◽  
Feature Size ◽  
Transmission Electron

AbstractThe demand for increasingly higher performance semiconductor products has stimulated the semiconductor industry to respond by producing devices with increasingly complex circuitry, more transistors in less space, more layers of metal, dielectric and interconnects, more interfaces, and a manufacturing process with nearly 1,000 steps. As all device features are shrunk in the quest for higher performance, the role of Transmission Electron Microscopy as a characterization tool takes on a continually increasing importance over older, lower-resolution characterization tools, such as SEM. The Ångstrom scale imaging resolution and nanometer scale chemical analysis and diffraction resolution provided by modem TEM's are particularly well suited for solving materials problems encountered during research, development, production engineering, reliability testing, and failure analysis. A critical enabling technology for the application of TEM to semiconductor based products as the feature size shrinks below a quarter micron is advances in specimen preparation. The traditional 1,000Å thick specimen will be unsatisfactory in a growing number of applications. It can be shown using a simple geometrical model, that the thickness of TEM specimens must shrink as the square root of the feature size reduction. Moreover, the center-targeting of these specimens must improve so that the centertargeting error shrinks linearly with the feature size reduction. To meet these challenges, control of the specimen preparation process will require a new generation of polishing and ion milling tools that make use of high resolution imaging to control the ion milling process. In addition, as the TEM specimen thickness shrinks, the thickness of surface amorphization produced must also be reduced. Gallium focused ion beam systems can produce hundreds of Ångstroms of amorphised surface silicon, an amount which can consume an entire thin specimen. This limitation to FIB milling requires a method of removal of amorphised material that leaves no artifact in the remaining material.

scholarly journals Sample Preparation Methodologies for In Situ Liquid and Gaseous Cell Analytical Transmission Electron Microscopy of Electropolished Specimens

2016 ◽  
Vol 22 (6) ◽  
pp. 1350-1359 ◽  
Author(s):  
Xiang Li Zhong ◽  
Sibylle Schilling ◽  
Nestor J. Zaluzec ◽  
M. Grace Burke
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
General Procedure ◽  
Ion Beam ◽  
Metals And Alloys ◽  
Stainless Steel Sample ◽  
Transmission Electron ◽  
Wide Range

AbstractIn recent years, an increasing number of studies utilizing in situ liquid and/or gaseous cell scanning/transmission electron microscopy (S/TEM) have been reported. Because of the difficulty in the preparation of suitable specimens, these environmental S/TEM studies have been generally limited to studies of nanoscale structured materials such as nanoparticles, nanowires, or sputtered thin films. In this paper, we present two methodologies which have been developed to facilitate the preparation of electron-transparent samples from conventional bulk metals and alloys for in situ liquid/gaseous cell S/TEM experiments. These methods take advantage of combining sequential electrochemical jet polishing followed by focused ion beam extraction techniques to create large electron-transparent areas for site-specific observation. As an example, we illustrate the application of this methodology for the preparation of in situ specimens from a cold-rolled Type 304 austenitic stainless steel sample, which was subsequently examined in both 1 atm of air as well as fully immersed in a H2O environment in the S/TEM followed by hyperspectral imaging. These preparation techniques can be successfully applied as a general procedure for a wide range of metals and alloys, and are suitable for a variety of in situ analytical S/TEM studies in both aqueous and gaseous environments.

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