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The oxidation of carbon nanostructures imaged by electron microscopy : Comparison between in-situ TEM and TGA experiments

Mases, Mattias ; Jacobsson, Daniel LU ; Wahlqvist, David LU ; Ek, Martin LU orcid and Wiinikka, Henrik (2024) In Applied Surface Science 672.
Abstract

The development of a model of carbon oxidation has engaged researchers for decades. Yet many outstanding questions remain due to the inability to experimentally study the details of the oxidation. Today, novel techniques such as environmental transmission electron microscopy (ETEM), allowing for in-situ nanoscale observations of the oxidation process, can help illuminate some of these questions. In this study of few layer graphene (FLG), multi-walled carbon nanotubes (MWCNTs), buckminsterfullerene (C60), and nanodiamonds (NDs) oxidizing in temperatures up to 1100 °C and we analyze the importance of nanostructure for the thermal stability of nanocarbons. The study was complemented with thermogravimetric analysis (TGA) and the... (More)

The development of a model of carbon oxidation has engaged researchers for decades. Yet many outstanding questions remain due to the inability to experimentally study the details of the oxidation. Today, novel techniques such as environmental transmission electron microscopy (ETEM), allowing for in-situ nanoscale observations of the oxidation process, can help illuminate some of these questions. In this study of few layer graphene (FLG), multi-walled carbon nanotubes (MWCNTs), buckminsterfullerene (C60), and nanodiamonds (NDs) oxidizing in temperatures up to 1100 °C and we analyze the importance of nanostructure for the thermal stability of nanocarbons. The study was complemented with thermogravimetric analysis (TGA) and the experiments were in good agreement with oxidation rates increasing sharply with temperature and the thermal stability of the materials MWCNTs, FLG, C60 and NDs in descending order. Based on the direct nanoscale visualization obtained in the ETEM the materials can be divided into two overall categories: materials with low strain sp2-bonds (FLG and MWCNT); and materials with high strain sp2-bonds (C60) or sp3-bonds (NDs). For materials in the first category, it is possible to identify several different phenomena as their oxidation rate increases as a function of temperatures whereas materials in the second category appear to be more influenced by extrinsic factors such as the electron beam and by structural transformation upon heating. This study clearly shows the value of adding ETEM results to traditional TGA investigations since it gives both a complementary and more detailed information about the dynamic oxidation process.

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author
; ; ; and
organization
publishing date
type
Contribution to journal
publication status
published
subject
keywords
Carbon nanostructures, DSC, ETEM, Oxidation, TGA
in
Applied Surface Science
volume
672
article number
160755
publisher
Elsevier
external identifiers
  • scopus:85199183947
ISSN
0169-4332
DOI
10.1016/j.apsusc.2024.160755
language
English
LU publication?
yes
id
07b79fb6-c9e4-45f8-ac1f-91967de04db9
date added to LUP
2024-09-03 13:36:02
date last changed
2024-09-09 13:34:50
@article{07b79fb6-c9e4-45f8-ac1f-91967de04db9,
  abstract     = {{<p>The development of a model of carbon oxidation has engaged researchers for decades. Yet many outstanding questions remain due to the inability to experimentally study the details of the oxidation. Today, novel techniques such as environmental transmission electron microscopy (ETEM), allowing for in-situ nanoscale observations of the oxidation process, can help illuminate some of these questions. In this study of few layer graphene (FLG), multi-walled carbon nanotubes (MWCNTs), buckminsterfullerene (C<sub>60</sub>), and nanodiamonds (NDs) oxidizing in temperatures up to 1100 °C and we analyze the importance of nanostructure for the thermal stability of nanocarbons. The study was complemented with thermogravimetric analysis (TGA) and the experiments were in good agreement with oxidation rates increasing sharply with temperature and the thermal stability of the materials MWCNTs, FLG, C<sub>60</sub> and NDs in descending order. Based on the direct nanoscale visualization obtained in the ETEM the materials can be divided into two overall categories: materials with low strain sp<sup>2</sup>-bonds (FLG and MWCNT); and materials with high strain sp<sup>2</sup>-bonds (C<sub>60</sub>) or sp<sup>3</sup>-bonds (NDs). For materials in the first category, it is possible to identify several different phenomena as their oxidation rate increases as a function of temperatures whereas materials in the second category appear to be more influenced by extrinsic factors such as the electron beam and by structural transformation upon heating. This study clearly shows the value of adding ETEM results to traditional TGA investigations since it gives both a complementary and more detailed information about the dynamic oxidation process.</p>}},
  author       = {{Mases, Mattias and Jacobsson, Daniel and Wahlqvist, David and Ek, Martin and Wiinikka, Henrik}},
  issn         = {{0169-4332}},
  keywords     = {{Carbon nanostructures; DSC; ETEM; Oxidation; TGA}},
  language     = {{eng}},
  publisher    = {{Elsevier}},
  series       = {{Applied Surface Science}},
  title        = {{The oxidation of carbon nanostructures imaged by electron microscopy : Comparison between in-situ TEM and TGA experiments}},
  url          = {{http://dx.doi.org/10.1016/j.apsusc.2024.160755}},
  doi          = {{10.1016/j.apsusc.2024.160755}},
  volume       = {{672}},
  year         = {{2024}},
}