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A multi-method study of the transformation of the carbonaceous skeleton of a polymer-based nanoporous carbon along the activation pathway

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posted on 08.09.2015 by Cheng Hu, Amelia C.Y. Liu, Matthew Weyland, S. Hadi Madani, Phillip Pendleton, Francisco Rodriguez-Reinoso, Katsumi Kaneko, Mark Biggs, L.A. Smillie
The change in the carbonaceous skeleton of nanoporous carbons during their activation has received limited attention, unlike its counterpart process in the presence of an inert atmosphere. Here we adopt a multi-method approach to elucidate this change in a poly(furfuryl alcohol)-derived carbon activated using cyclic application of oxygen saturation at 250 °C before its removal (with carbon) at 800 °C in argon. The methods used include helium pycnometry, synchrotron-based X-ray diffraction (XRD) and associated radial distribution function (RDF) analysis, transmission electron microscopy (TEM) and, uniquely, electron energy-loss spectroscopy spectrum-imaging (EELS-SI), electron nanodiffraction and fluctuation electron microscopy (FEM). Helium pycnometry indicates the solid skeleton of the carbon densifies during activation from 78% to 93% of graphite. RDF analysis, EELS-SI, and FEM all suggest this densification comes through an in-plane growth of sp2 carbon out to the medium range without commensurate increase in order normal to the plane. This process could be termed ‘graphenization’. The exact way in which this process occurs is not clear, but TEM images of the carbon before and after activation suggest it may come through removal of the more reactive carbon, breaking constraining cross-links and creating space that allows the remaining carbon material to migrate in an annealing-like process.

Funding

C.H. acknowledges a joint scholarship provided by China Scholarship Council (CSC) and the University of Adelaide. The support of the Australian Research Council Discovery Program (DP110101293) is also gratefully acknowledged. ACYL gratefully acknowledges the support of the Science Faculty and the Monash Centre for Electron Microscopy (MCEM), Monash University. The electron microscopy was performed in the MCEM. The FEI Titan3 80-300 FEGTEM was funded by the Australian Research Council (LE0454166). S.H.M. acknowledges the award of a President’s Scholarship from the University of South Australia.

History

School

  • Science

Department

  • Chemistry

Published in

CARBON

Volume

85

Pages

119 - 134 (16)

Citation

HU, C. ... et al, 2015. A multi-method study of the transformation of the carbonaceous skeleton of a polymer-based nanoporous carbon along the activation pathway. Carbon, 85, pp. 119 - 134.

Publisher

© Elsevier Ltd

Version

AM (Accepted Manuscript)

Publisher statement

This work is made available according to the conditions of the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International (CC BY-NC-ND 4.0) licence. Full details of this licence are available at: https://creativecommons.org/licenses/by-nc-nd/4.0/

Publication date

2015

Notes

This article was published in the journal, Carbon [© Elsevier] and the definitive version is available at: http://dx.doi.org/10.1016/j.carbon.2014.12.051 . This manuscript version is made available under the CC-BY-NC-ND 4.0 licensehttp://creativecommons.org/licenses/by-nc-nd/4.0/

ISSN

0008-6223

Language

en

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