Transmission electron microscopy investigations of (hydrous) chain silicates from the lithospheric mantle beneath the Carpathian Pannonian Region

Author(s):  
Zsófia Pálos ◽  
Péter Pekker ◽  
Mihály Pósfai ◽  
Thomas Pieter Lange ◽  
Nóra Liptai ◽  
...  

<p>Transmission electron microscopy (TEM) is a powerful, yet scarcely used technique when it comes to investigating mantle minerals and fluid inclusions. It is capable to collect structural information of the studied mineral, its precise chemical composition, and makes nanofeatures visible, such as dislocations and nano-inclusions.</p><p>In this study TEM and STEM (scanning transmission electron microscopy) measurements were carried out on a set of ortho- and clinopyroxene samples from central and marginal localities of Carpathian Pannonian region (CPR), where Plio-Pleistocene alkaline basalt volcanism sampled the lithospheric mantle retrieving lithospheric mantle xenoliths. Objective of the study was to constrain the presence and formation mechanisms of sub-microscopic occurrence of pargasitic amphibole.</p><p>The detailed investigation of pargasite in the upper mantle is rather timely, because its presence may be the major cause for the rheologic contrast experienced between the lithosphere and the asthenosphere [1], [2]. The nominally anhydrous minerals’ (NAMs, as ortho- and clinopyroxene) structural hydroxyl [3] content or volatiles in fluid inclusions could lead to formation of pargasite [4]. In addition, pargasite could form interstitially during metasomatic intereactions.</p><p>Our observations so far suggest that hydrous silicate formation as sub-solidus exsolution in the central CPR may not have taken place. Ordering of the Ca forming Ca-rich and Ca-poor domains in an orthopyroxene grain was identified. Precursors of H<sup>+</sup> diffusion were also recorded, such as dislocations and nanosized fluid inclusions. Diffusion of H<sup>+</sup> could be active in the lattice scale through the disclinations along subgrain boundaries [3], [5] or dislocations in the host mineral along the boundary of nanoscale fluid inclusions [6], [7]. Clinopyroxene-amphibole phase boundary has been prepared by focused ion beam (FIB) milling technique from the marginal area of CPR. The chemical composition of the amphibole lamella provides evidence that the H<sub>2</sub>O content of the nearby fluid inclusion migrated into the host clinopyroxene producing an amphibole lamella growing along the ‘c’ crystallographic axis [4].</p><p>Observations of the boundary of clinopyroxene and amphibole confirm that the amphibole octahedral layers penetrate the clinopyroxene structure. The precise nanoscale measurements (STEM mapping) of chemical composition of both the host and the lamellae can lead to profound implications on the original composition of the studied fluid inclusions.</p><p>[1] Green, D. H., Hibberson, W. O., Kovács, I. J., & Rosenthal, A. (2010). <em>Nature</em>, 467(7314), 448–451.</p><p>[2] Kovács, I. J., Lenkey, L., Green, D. H., Fancsik, T., Falus, G., Kiss, J., Orosz, L., Angyal, J., Vikor, Zs. (2017). <em>Acta Geodaetica et Geophysica</em>, 52, 183–204.</p><p>[3] Liptai, N., Kovács, I.J., Lange, T.P., Pálos, Zs., Berkesi, M., Szabó, Cs., Wesztergom, V. (2019). <em>Goldschmidt Abstracts</em>, 2019 1981.</p><p>[4] Lange, T.P., Liptai, N., Patkó, L., Berkesi, M., Kesjár, D., Szabó, Cs., Kovács, I. J. (2019). 25th European Current Research on Fluid Inclusions (ECROFI) , <em>Abstract Series</em>, 68.</p><p>[5] Demouchy, S., & Bolfan-Casanova, N. (2016). <em>Lithos</em>, 240–243, 402–425.</p><p>[6] Bakker, R. J., & Jansen, J. B. H. (1994). <em>Contributions to Mineralogy and Petrology</em>, 116, 7–20.</p><p>[7] Viti, C., & Frezzotti, M. L. (2000). <em>American Mineralogist</em>, 85(10), 1390–1396.</p>

Author(s):  
George Guthrie ◽  
David Veblen

The nature of a geologic fluid can often be inferred from fluid-filled cavities (generally <100 μm in size) that are trapped during the growth of a mineral. A variety of techniques enables the fluids and daughter crystals (any solid precipitated from the trapped fluid) to be identified from cavities greater than a few micrometers. Many minerals, however, contain fluid inclusions smaller than a micrometer. Though inclusions this small are difficult or impossible to study by conventional techniques, they are ideally suited for study by analytical/ transmission electron microscopy (A/TEM) and electron diffraction. We have used this technique to study fluid inclusions and daughter crystals in diamond and feldspar.Inclusion-rich samples of diamond and feldspar were ion-thinned to electron transparency and examined with a Philips 420T electron microscope (120 keV) equipped with an EDAX beryllium-windowed energy dispersive spectrometer. Thin edges of the sample were perforated in areas that appeared in light microscopy to be populated densely with inclusions. In a few cases, the perforations were bound polygonal sides to which crystals (structurally and compositionally different from the host mineral) were attached (Figure 1).


Author(s):  
Ching Shan Sung ◽  
Hsiu Ting Lee ◽  
Jian Shing Luo

Abstract Transmission electron microscopy (TEM) plays an important role in the structural analysis and characterization of materials for process evaluation and failure analysis in the integrated circuit (IC) industry as device shrinkage continues. It is well known that a high quality TEM sample is one of the keys which enables to facilitate successful TEM analysis. This paper demonstrates a few examples to show the tricks on positioning, protection deposition, sample dicing, and focused ion beam milling of the TEM sample preparation for advanced DRAMs. The micro-structures of the devices and samples architectures were observed by using cross sectional transmission electron microscopy, scanning electron microscopy, and optical microscopy. Following these tricks can help readers to prepare TEM samples with higher quality and efficiency.


Author(s):  
K. Doong ◽  
J.-M. Fu ◽  
Y.-C. Huang

Abstract The specimen preparation technique using focused ion beam (FIB) to generate cross-sectional transmission electron microscopy (XTEM) samples of chemical vapor deposition (CVD) of Tungsten-plug (W-plug) and Tungsten Silicides (WSix) was studied. Using the combination method including two axes tilting[l], gas enhanced focused ion beam milling[2] and sacrificial metal coating on both sides of electron transmission membrane[3], it was possible to prepare a sample with minimal thickness (less than 1000 A) to get high spatial resolution in TEM observation. Based on this novel thinning technique, some applications such as XTEM observation of W-plug with different aspect ratio (I - 6), and the grain structure of CVD W-plug and CVD WSix were done. Also the problems and artifacts of XTEM sample preparation of high Z-factor material such as CVD W-plug and CVD WSix were given and the ways to avoid or minimize them were suggested.


Author(s):  
Chin Kai Liu ◽  
Chi Jen. Chen ◽  
Jeh Yan.Chiou ◽  
David Su

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.


Materials ◽  
2021 ◽  
Vol 14 (6) ◽  
pp. 1431
Author(s):  
Seiichiro Ii ◽  
Takero Enami ◽  
Takahito Ohmura ◽  
Sadahiro Tsurekawa

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.


2010 ◽  
Vol 16 (6) ◽  
pp. 662-669 ◽  
Author(s):  
S. Simões ◽  
F. Viana ◽  
A.S. Ramos ◽  
M.T. Vieira ◽  
M.F. Vieira

AbstractReactive multilayer thin films that undergo highly exothermic reactions are attractive choices for applications in ignition, propulsion, and joining systems. Ni/Al reactive multilayer thin films were deposited by dc magnetron sputtering with a period of 14 nm. The microstructure of the as-deposited and heat-treated Ni/Al multilayers was studied by transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) in plan view and in cross section. The cross-section samples for TEM and STEM were prepared by focused ion beam lift-out technique. TEM analysis indicates that the as-deposited samples were composed of Ni and Al. High-resolution TEM images reveal the presence of NiAl in small localized regions. Microstructural characterization shows that heat treating at 450 and 700°C transforms the Ni/Al multilayered structure into equiaxed NiAl fine grains.


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.


Sign in / Sign up

Export Citation Format

Share Document