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Robust Sample Preparation of Large-Area In- and Out-of-Plane Cross Sections of Layered Materials with Ultramicrotomy
[Image: see text] Layered materials (LMs) such as graphene or MoS(2) have attracted a great deal of interest recently. These materials offer unique functionalities due to their structural anisotropy characterized by weak van der Waals bonds along the out-of-plane axis and covalent bonds in the in-pl...
Autores principales: | , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
American
Chemical Society
2020
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Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7118708/ https://www.ncbi.nlm.nih.gov/pubmed/32155046 http://dx.doi.org/10.1021/acsami.9b22586 |
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author | Cichocka, Magdalena O. Bolhuis, Maarten van Heijst, Sabrya E. Conesa-Boj, Sonia |
author_facet | Cichocka, Magdalena O. Bolhuis, Maarten van Heijst, Sabrya E. Conesa-Boj, Sonia |
author_sort | Cichocka, Magdalena O. |
collection | PubMed |
description | [Image: see text] Layered materials (LMs) such as graphene or MoS(2) have attracted a great deal of interest recently. These materials offer unique functionalities due to their structural anisotropy characterized by weak van der Waals bonds along the out-of-plane axis and covalent bonds in the in-plane direction. A central requirement to access the structural information on complex nanostructures built upon LMs is to control the relative orientation of each sample prior to their inspection, e.g., with transmission electron microscopy (TEM). However, developing sample preparation methods that result in large inspection areas and ensure full control over the sample orientation while avoiding damage during the transfer to the TEM grid is challenging. Here, we demonstrate the feasibility of deploying ultramicrotomy for the preparation of LM samples in TEM analyses. We show how ultramicrotomy leads to the reproducible large-scale production of both in-plane and out-of-plane cross sections, with bulk vertically oriented MoS(2) and WS(2) nanosheets as a proof of concept. The robustness of the prepared samples is subsequently verified by their characterization by means of both high-resolution TEM and Raman spectroscopy measurements. Our approach is fully general and should find applications for a wide range of materials as well as of techniques beyond TEM, thus paving the way to the systematic large-area mass-production of cross-sectional specimens for structural and compositional studies. |
format | Online Article Text |
id | pubmed-7118708 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2020 |
publisher | American
Chemical Society |
record_format | MEDLINE/PubMed |
spelling | pubmed-71187082020-04-03 Robust Sample Preparation of Large-Area In- and Out-of-Plane Cross Sections of Layered Materials with Ultramicrotomy Cichocka, Magdalena O. Bolhuis, Maarten van Heijst, Sabrya E. Conesa-Boj, Sonia ACS Appl Mater Interfaces [Image: see text] Layered materials (LMs) such as graphene or MoS(2) have attracted a great deal of interest recently. These materials offer unique functionalities due to their structural anisotropy characterized by weak van der Waals bonds along the out-of-plane axis and covalent bonds in the in-plane direction. A central requirement to access the structural information on complex nanostructures built upon LMs is to control the relative orientation of each sample prior to their inspection, e.g., with transmission electron microscopy (TEM). However, developing sample preparation methods that result in large inspection areas and ensure full control over the sample orientation while avoiding damage during the transfer to the TEM grid is challenging. Here, we demonstrate the feasibility of deploying ultramicrotomy for the preparation of LM samples in TEM analyses. We show how ultramicrotomy leads to the reproducible large-scale production of both in-plane and out-of-plane cross sections, with bulk vertically oriented MoS(2) and WS(2) nanosheets as a proof of concept. The robustness of the prepared samples is subsequently verified by their characterization by means of both high-resolution TEM and Raman spectroscopy measurements. Our approach is fully general and should find applications for a wide range of materials as well as of techniques beyond TEM, thus paving the way to the systematic large-area mass-production of cross-sectional specimens for structural and compositional studies. American Chemical Society 2020-03-10 2020-04-01 /pmc/articles/PMC7118708/ /pubmed/32155046 http://dx.doi.org/10.1021/acsami.9b22586 Text en Copyright © 2020 American Chemical Society This is an open access article published under a Creative Commons Non-Commercial No Derivative Works (CC-BY-NC-ND) Attribution License (http://pubs.acs.org/page/policy/authorchoice_ccbyncnd_termsofuse.html) , which permits copying and redistribution of the article, and creation of adaptations, all for non-commercial purposes. |
spellingShingle | Cichocka, Magdalena O. Bolhuis, Maarten van Heijst, Sabrya E. Conesa-Boj, Sonia Robust Sample Preparation of Large-Area In- and Out-of-Plane Cross Sections of Layered Materials with Ultramicrotomy |
title | Robust
Sample Preparation of Large-Area In- and Out-of-Plane
Cross Sections of Layered Materials with Ultramicrotomy |
title_full | Robust
Sample Preparation of Large-Area In- and Out-of-Plane
Cross Sections of Layered Materials with Ultramicrotomy |
title_fullStr | Robust
Sample Preparation of Large-Area In- and Out-of-Plane
Cross Sections of Layered Materials with Ultramicrotomy |
title_full_unstemmed | Robust
Sample Preparation of Large-Area In- and Out-of-Plane
Cross Sections of Layered Materials with Ultramicrotomy |
title_short | Robust
Sample Preparation of Large-Area In- and Out-of-Plane
Cross Sections of Layered Materials with Ultramicrotomy |
title_sort | robust
sample preparation of large-area in- and out-of-plane
cross sections of layered materials with ultramicrotomy |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7118708/ https://www.ncbi.nlm.nih.gov/pubmed/32155046 http://dx.doi.org/10.1021/acsami.9b22586 |
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