Reply to the comments of Y.H. Liu: Ion sputter erosion in metallic glass—A response to “Comment on: Homogeneity of Zr64.13Cu15.75Ni10.12Al10 bulk metallic glass” by L-Y. Chen, Y-W. Zeng, Q-P. Cao, B-J. Park, Y-M. Chen, K. Hono, U. Vainio, Z-L. Zhang, U. Kaiser, X-D. Wang,and J-Z Jiang [J. Mater. Res. 24, 3116 (2009)]

2010 ◽  
Vol 25 (3) ◽  
pp. 602-604 ◽  
Author(s):  
Lian-Yi Chen ◽  
Qing-Ping Cao ◽  
J.Z. Jiang ◽  
Jing-Wei Deng

The morphology of the dark and bright regions observed by transmission electron microscopy for the Zr64.13Cu15.75Ni10.12Al10 bulk metallic glass strongly depends on the ion beam parameters used for ion milling. This indicates that the ion beam could introduce surface fluctuation to metallic glasses during ion milling.

2013 ◽  
Vol 774-776 ◽  
pp. 799-802
Author(s):  
Zhong Yuan Liu ◽  
J. Tan ◽  
G. Wang

In this paper, high resolution transmission electron microscopy (HRTEM) has been used to observe a Zr41.25Ti13.75Ni10Cu12.5Be22.5 (at. %) bulk metallic glass (BMG) prepared from different methods, i.e. ion milling and electropolishing. The ion thinning brings out the white bulb pattern on the specimen surface and induces localized temperature increasing. The electropolishing does not influence microstructure of the amorphous phase. A new preparation technique of grinding method is introduced. For BMG, the electropolishing and grinding are the better method for TEM specimen preparation as compared with the ion thinning.


1998 ◽  
Vol 523 ◽  
Author(s):  
John Mardinly ◽  
David W. Susnitzky

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.


Author(s):  
Ngee-Sing Chong ◽  
Michael L. Norton

Existing techniques for the preparation of metallic specimens for examination by transmission electron microscopy consist primarily of jet electrolysis or ion milling. Both of these procedures are well-established and are suitable for thinning metallic specimens of interests from a thickness of 0.1 mm to 30-100 nm. Despite its popularity, the former technique may not be suitable for thinning electrodeposited films of 1-5 um thick because of its rather rapid thinning rate of 0.5-1.0 um/sec. Furthermore, it is difficult to ensure good electrical contact between such a delicate film and the specimen holder. Hence, the older method of “window” electropolishing may be applicable owing to its slower thinning rate despite the troublesome steps of lacquering specimen edges, finding suitable polishing conditions, and making electrical attachment. Ion milling, despite its relatively high cost, may be suitable for thinning the nickel films because of its slow milling rates on the order of 110 um/hr. However, special expertise is required in the manipulation of milling conditions such as ion energy and incident ion beam angle to avoid creating the structural artifacts of ion implantation, atom translocation, and bubbling.


2009 ◽  
Vol 24 (1) ◽  
pp. 1-9 ◽  
Author(s):  
Y.M. Chen ◽  
T. Ohkubo ◽  
T. Mukai ◽  
K. Hono

The atomic structure of shear bands in Pd40Ni40P20 bulk metallic glass has been compared to an undeformed matrix phase using pair distribution functions (PDFs) derived from energy filtered nanobeam electron diffraction. Shear bands do not show any characteristic contrast in transmission electron microscopy (TEM) images when specimens are prepared with uniform thickness. PDFs from a shear band exhibit a slight decrease in the first peak, indicating a slight difference in packing density and short range order compared to the undeformed matrix.


2003 ◽  
Vol 9 (6) ◽  
pp. 509-515 ◽  
Author(s):  
Jing Li ◽  
X. Gu ◽  
T.C. Hufnagel

We have used fluctuation microscopy to reveal the presence of structural order on length scales of 1–2 nm in metallic glasses. We compare results of fluctuation microscopy measurements with high resolution transmission electron microscopy and electron diffraction observations on a series of metallic glass samples with differing degrees of structural order. The agreement between the fluctuation microscopy results and those of the other techniques is good. In particular, we show that the technique used to make thin specimens for electron microscopy affects the structure of the metallic glass, with ion thinning inducing more structural order than electropolishing. We also show that relatively minor changes in the composition of the alloy can have a significant effect on the medium-range order; this increased order is correlated with changes in mechanical behavior.


1997 ◽  
Vol 480 ◽  
Author(s):  
Jeong Soo Lee ◽  
Hyun Ha Kim ◽  
Young Woo Jeong

AbstractThe cross-sectional transmission electron microscopy (TEM) specimens of Pt/Ti/SiO2/Si, RuO2/SiO2/Si, W/TiN/SiO2/Si, (Pb,La)TiO3/Pt/MgO, Bi4Ti3O12/Lal-xCaxMnO3/MgO, and GaN/Al2O3 were successfully made by the rocking-angle ion-milling technique. The differential thinning problems could be effectively mitigated when the rocking-angle and the ion-beam incidence angle were optimized for each heterostructure. It was found that the sputtering yield ratio between the layer milled most quickly and the layer milled most slowly is one of the important factors which determine the optimum rocking-angle ion-milling condition. The atomic force microscopy study on the surface topography of the cross-sectional Pt/Ti/SiO2/Si TEM sample after ion-milling provided quantitative information about the effects of the rocking-angle variation. A parameter which is the ratio between the layer with a minimum electron transparency and the layer with a maximum electron transparency was suggested.


2010 ◽  
Vol 25 (3) ◽  
pp. 598-601 ◽  
Author(s):  
Yanhui Liu ◽  
Wei H. Wang

In a recent work, Chen et al. [L-Y. Chen et al., J. Mater. Res.24, 3116 (2009)] presented microstructural observation on a plastic Zr64.13Cu15.75Ni10.12Al10 bulk metallic glass (BMG) reported in Liu et al. [Y.H. Liu et al., Science315, 1385 (2007)] by using transmission electron microscopy (TEM) and anomalous small-angle x-ray scattering experiments. Based on their observation, they draw a conclusion that there are no micrometer-sized or nanometer-sized structural heterogeneities in the BMG, and the large plasticity of the BMG cannot be ascribed to the structural heterogeneities. In this comment, we show that their assessment and analysis of their observation are problematic, and it is not evident and precise to use their observation to claim that the BMG is homogeneous and the structural heterogeneity in the glass is an artifact.


2020 ◽  
Vol 50 (1) ◽  
Author(s):  
Yena Kwon ◽  
Byeong-Seon An ◽  
Yeon-Ju Shin ◽  
Cheol-Woong Yang

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.


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