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Title: Studies of reaction mechanisms during stabilization of electrospun polyacrylonitrile carbon nanofibers

Abstract

Various reaction mechanisms such as cyclization, oxidation, dehydrogenation, and crosslinking are studied during stabilization of electrospun polyacrylonitrile nanofibers using different in situ techniques such as differential scanning calorimetry (DSC), shrinkage measurement, and dynamic mechanical analysis (DMA). DSC results show that oxidation preferentially occurs in cyclized structure. It is also found that the cyclization reaction has the highest activation energy followed by oxidation/dehydrogenation and crosslinking reactions. In situ shrinkage measurement and DMA data are used to study the extent of cyclization and cross-linking reactions, respectively, in air. Comparing the in situ shrinkage measurement with DSC data, it is found that cyclization reaction in air progresses in two different mechanisms such as radical cyclization, which depends only on the temperature and ionic cyclization, which is limited by the rate of oxygen diffusion. In conclusion, it is found that complete cyclization time occurs at about 189 min for isothermal heat treatment at 260 °C with 5 °C/min ramp, while cross-linking reaction becomes dominant at 132 min.

Authors:
 [1]; ORCiD logo [2]
  1. Argonne National Lab. (ANL), Lemont, IL (United States)
  2. Univ. of Oklahoma, Norman, OK (United States)
Publication Date:
Research Org.:
Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Org.:
University of Oklahoma; USDOE Office of Science (SC)
OSTI Identifier:
1489823
Grant/Contract Number:  
AC02-06CH11357
Resource Type:
Accepted Manuscript
Journal Name:
Polymer Engineering and Science
Additional Journal Information:
Journal Volume: 58; Journal Issue: 8; Journal ID: ISSN 0032-3888
Publisher:
Wiley
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; carbon nanofiber; cyclization; electrospinning; polyacrylonitrile; stabilization

Citation Formats

Barua, Bipul, and Saha, Mrinal C. Studies of reaction mechanisms during stabilization of electrospun polyacrylonitrile carbon nanofibers. United States: N. p., 2017. Web. doi:10.1002/pen.24708.
Barua, Bipul, & Saha, Mrinal C. Studies of reaction mechanisms during stabilization of electrospun polyacrylonitrile carbon nanofibers. United States. doi:10.1002/pen.24708.
Barua, Bipul, and Saha, Mrinal C. Fri . "Studies of reaction mechanisms during stabilization of electrospun polyacrylonitrile carbon nanofibers". United States. doi:10.1002/pen.24708. https://www.osti.gov/servlets/purl/1489823.
@article{osti_1489823,
title = {Studies of reaction mechanisms during stabilization of electrospun polyacrylonitrile carbon nanofibers},
author = {Barua, Bipul and Saha, Mrinal C.},
abstractNote = {Various reaction mechanisms such as cyclization, oxidation, dehydrogenation, and crosslinking are studied during stabilization of electrospun polyacrylonitrile nanofibers using different in situ techniques such as differential scanning calorimetry (DSC), shrinkage measurement, and dynamic mechanical analysis (DMA). DSC results show that oxidation preferentially occurs in cyclized structure. It is also found that the cyclization reaction has the highest activation energy followed by oxidation/dehydrogenation and crosslinking reactions. In situ shrinkage measurement and DMA data are used to study the extent of cyclization and cross-linking reactions, respectively, in air. Comparing the in situ shrinkage measurement with DSC data, it is found that cyclization reaction in air progresses in two different mechanisms such as radical cyclization, which depends only on the temperature and ionic cyclization, which is limited by the rate of oxygen diffusion. In conclusion, it is found that complete cyclization time occurs at about 189 min for isothermal heat treatment at 260 °C with 5 °C/min ramp, while cross-linking reaction becomes dominant at 132 min.},
doi = {10.1002/pen.24708},
journal = {Polymer Engineering and Science},
number = 8,
volume = 58,
place = {United States},
year = {2017},
month = {9}
}

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Works referenced in this record:

A review on polymer nanofibers by electrospinning and their applications in nanocomposites
journal, November 2003

  • Huang, Zheng-Ming; Zhang, Y.-Z.; Kotaki, M.
  • Composites Science and Technology, Vol. 63, Issue 15, p. 2223-2253
  • DOI: 10.1016/S0266-3538(03)00178-7